Ultrasonic Assisted Extraction of Artemisinin from Artemisia Annua L. Using Monoether based Solvents

PROCESS Comments Off

Dec 252017

Artemisia Annua L

Ultrasonic Assisted Extraction of Artemisinin from Artemisia Annua L. Using Monoether based Solvents

Yongqiang Zhang, Phongphat Prawang, CHUNSHAN LI, Xiangzhan Meng, Yu Zhao, Hui Wang and Suojiang Zhang

Abstract

Artemisinin is a kind of natural antimalarial drug exhibiting low toxicity with a very fast action against malaria. Solvent extraction is the most widely used method to separate artemisinin from the Chinese medicinal herb Artemisia annua L. In this study, a series of monoether based solvents have been proposed to extract artemisinin and propylene glycol methyl ether (PGME) was found to be the most appropriate one for this extraction. Ultrasonic irradiation was demonstrated to be able to assist artemisinin extraction. Influences of extraction conditions, including liquid/solid ratio, extraction temperature, ultrasonic time, ultrasonic power, on the extraction efficiency were discussed by single factor experiments, and the main influence factors were optimized by responds surface method. The extraction mechanism was explored with spectroscopic characterizations, and kinetics of this process was also studied. Results indicate that ultrasonic assisted extraction using PGME has faster extraction rate than conventional solvents, and ultrasonic can significantly enhance mass transfer. Compared with conventional extraction, the process developed here exhibited higher efficiency (13.79 mg/g vs. 13.29 mg/g) and short extraction time (decreased from 8 h to 0.5 h) at a relatively low temperature. In addition, PGME has low toxicity and volatility, making the extraction process more safe and reliable. Therefore, this proposed method demonstrates that PGME based ultrasonic assisted extraction is a rapid, efficient, simple and safe technique for natural product extraction.

http://pubs.rsc.org/en/Content/ArticleLanding/2017/GC/C7GC03191B?utm_source=feedburner&utm_medium=feed&utm_campaign=Feed%3A+rss%2FGC+%28RSC+-+Green+Chem.+latest+articles%29#!divAbstract

/////////// Artemisinin, Artemisia Annua L, extraction

HMF in multicomponent reactions: utilization of 5-hydroxymethylfurfural (HMF) in the Biginelli reaction

organic chemistry, spectroscopy, SYNTHESIS Comments Off

Dec 212017

HMF in multicomponent reactions: utilization of 5-hydroxymethylfurfural (HMF) in the Biginelli reaction

Green Chem., 2018, Advance Article
DOI: 10.1039/C7GC03425C, Paper

Weigang Fan, Yves Queneau, Florence Popowycz
The use of the renewable platform molecule 5-hydroxymethylfurfural (HMF) in the multi-component Biginelli reaction has been investigated.

HMF in multicomponent reactions: utilization of 5-hydroxymethylfurfural (HMF) in the Biginelli reaction

Weigang Fan,^a Yves Queneau*^a and Florence Popowycz*^a

http://pubs.rsc.org/en/Content/ArticleLanding/2018/GC/C7GC03425C?utm_source=feedburner&utm_medium=feed&utm_campaign=Feed%3A+rss%2FGC+%28RSC+-+Green+Chem.+latest+articles%29#!divAbstract

* Corresponding authors

^a Université de Lyon, INSA Lyon, ICBMS, Equipe Chimie Organique et Bioorganique, UMR 5246 CNRS, Université Lyon 1, CPE Lyon, Bâtiment Jules Verne, 20 Avenue Albert Einstein, F-69621 Villeurbanne Cedex, France
E-mail: yves.queneau@insa-lyon.fr, florence.popowycz@insa-lyon.fr

Abstract

The use of the renewable platform molecule 5-hydroxymethylfurfural (HMF) in the multi-component Biginelli reaction has been investigated. Multicomponent reactions (MCR) using HMF offer straightforward access to novel fine chemicals. However, the peculiar reactivity and lower stability of HMF have limited its use in such strategies. In this paper, we report our results on the use of HMF in 3-component Biginelli reactions, leading in one single step to a series of functionalized dihydropyrimidinones obtained in moderate to good yields, with a broad substrate scope of 1,3-dicarbonyl compounds and urea building blocks. This is the first report on the use of HMF in this reaction. The CH₂OH motif found in HMF provides useful functionalization for the target molecules, which cannot be offered by simpler aldehydes such as furfural.

5-Acetyl-4-[5’-(hydroxymethyl)furan-2’-yl]-6-methyl-3,4-dihydropyrimidin-2(1H)-one (4a):

Reaction time: 8 h; Global yield: 86%; (78% yield after simple filtration + additional 8% yield after purification of the filtrate by column chromatography).

1H NMR (400 MHz, DMSO-d6) δ 9.22 (d, 1H, J = 1.2 Hz, H1), 7.88 (dd, 1H, J = 3.4, 1.2 Hz, H3), 6.16 (d, 1H, J = 3.1 Hz, H4’), 6.03 (d, 1H, J = 3.1 Hz, H3’), 5.27 (d, 1H, J = 3.4 Hz, H4), 5.18 (t, 1H, J = 5.6 Hz, OH), 4.33 (d, 2H, J = 5.6 Hz, CH2), 2.25 (s, 3H, CH3-C6), 2.17 (s, 3H, CH3CO).

13C NMR (100 MHz, DMSO-d6) δ 193.9 (COCH3), 155.1, 154.9 (C2’, C5’), 152.4 (C2), 149.0 (C6), 107.7 (C4’), 107.1 (C5), 106.3 (C3’), 55.7 (CH2OH), 47.9 (C4), 30.0 (CH3CO), 19.0 (CH3-C6).

HRMS (ESI) m/z: Calcd for [M+Na]+ C12H14N2NaO4 273.0846; Found 273.0850.

Weigang Fan

Research experience

Sep 2015–Mar 2017

Doctorant

Institut National des Sciences Appliquées de Lyon · Institut de Chimie et de Biochimie Moléculaires et Supramoléculaires (ICBMS – UMR 5246)

France · Lyon

Florence POPOWYCZ

Université de Lyon, INSA Lyon, ICBMS, Equipe Chimie Organique et Bioorganique, UMR 5246 CNRS, Université Lyon 1, CPE Lyon, Bâtiment Jules Verne, 20 Avenue Albert Einstein, F-69621 Villeurbanne Cedex, France
E-mail: florence.popowycz@insa-lyon.fr

Yves QUENEAU

CNRS Research Director chez ICBMS INSA Lyon Univ Lyon – Carbohydrate Chemistry

ICBMS INSA Lyon University of Lyon

///////////////HMF, multicomponent reactions, 5-hydroxymethylfurfural, Biginelli reaction

Synthesis of highly functional carbamates through ring-opening of cyclic carbonates with unprotected α-amino acids in water

organic chemistry, spectroscopy, SYNTHESIS Comments Off

Dec 202017

Synthesis of highly functional carbamates through ring-opening of cyclic carbonates with unprotected [small alpha]-amino acids in water

Green Chem., 2018, Advance Article
DOI: 10.1039/C7GC02862H, Paper

Peter Olsen, Michael Oschmann, Eric V. Johnston, Bjorn Akermark
Ring opening of cyclic carbonates with unprotected amino acids in water – a route to highly functional carbamates.

Synthesis of highly functional carbamates through ring-opening of cyclic carbonates with unprotected α-amino acids in water

Peter Olsén,*^a Michael Oschmann,^a Eric V. Johnston*^a and Björn Åkermark*^a

Author affiliations

*Corresponding authors

^aDepartment of Organic Chemistry, Arrhenius Laboratory, Stockholm University, SE 106 91, Stockholm, Sweden
E-mail: peter.olsen@su.se, eric@sigridthx.com, bjorn.akermark@su.se

Abstract

The present work shows that it is possible to ring-open cyclic carbonates with unprotected amino acids in water. Fine tuning of the reaction parameters made it possible to suppress the degree of hydrolysis in relation to aminolysis. This enabled the synthesis of functionally dense carbamates containing alkenes, carboxylic acids, alcohols and thiols after short reaction times at room temperature. When Glycine was used as the nucleophile in the ring-opening with four different five membered cyclic carbonates, containing a plethora of functional groups, the corresponding carbamates could be obtained in excellent yields (>90%) without the need for any further purification. Furthermore, the orthogonality of the transformation was explored through ring-opening of divinylenecarbonate with unprotected amino acids equipped with nucleophilic side chains, such as serine and cysteine. In these cases the reaction selectively produced the desired carbamate, in 70 and 50% yield respectively. The synthetic design provides an inexpensive and scalable protocol towards highly functionalized building blocks that are envisioned to find applications in both the small and macromolecular arena.

link http://pubs.rsc.org/en/Content/ArticleLanding/2018/GC/C7GC02862H?utm_source=feedburner&utm_medium=feed&utm_campaign=Feed%3A+rss%2FGC+%28RSC+-+Green+Chem.+latest+articles%29#!divAbstract

Affiliation

Stockholm University

Location

Stockholm, Sweden

Department

Department of Organic Chemistry

Position

PostDoc Position

Research experience

Jun 2010–Feb 2016

PhD Student

KTH Royal Institute of Technology · Department of Fibre and Polymer Technology

Sweden · Stockholm

Björn Åkermark

Education

Jan 1962–Jun 1967

KTH Royal Institute of Technology

Organic Chemistry and Catalysis · PhD

Sweden · Stockholm

Awards & achievements

Jun 2009

Award: Bror Holmberg Medal, Swedish Chemical Society
Feb 2009

Award: Ulla and Stig Holmquists Prize, Uppsala University
Oct 1997

Award: Dr hc, University D´Aix-Marseille
Oct 1991

Award: KTH Prize for Excellence in Teaching
Oct 1978

Award: Arrhenius Medal, Swedish Chemical Society
Aug 1977

Scholarship: Zorn Fellowship, Swden America Foundation
Nov 1976

Award: Letterstedt Award, Roy Swed. Acad. of Science

Dr. Eric Johnston, Ph.D.

Chief Technology Officer

Dr. Eric V. Johnston obtained his Master of Science degree in 2008 at the Department of Organic Chemistry, Stockholm University, Sweden. In the same year, he started his graduate studies under the supervision of Prof. Jan-Erling Bäckvall. During his PhD, he worked on the development of new homogeneous and heterogeneous transition-metal catalysts.

After receiving his PhD in 2012, he joined Prof. Samuel J. Danishefskys research group at Memorial Sloan-Kettering Cancer Center, New York, USA as a postdoctoral fellow supported by The Swedish Research Council. Here he was engaged in the total chemical synthesis of glycolsylated proteins that play important roles in modern cancer treatment.

In 2014 he returned to the Department of Organic Chemistry at Stockholm University to establish his own group. The goal of his research is to contribute new advances to the strategy and methodology for the preparation of synthetic macromolecules such as proteins, glycopeptides, sequence and length-controlled polymers. He is also a Co-Supervisor for Prof. Björn Åkermarks research group, which aims at studying and developing new homogeneous, as well as heterogeneous, water oxidation catalysts.

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Applications and perspectives of nanomaterials in novel vaccine development

nanotechnology, VACCINE Comments Off

Dec 112017

Applications and perspectives of nanomaterials in novel vaccine development

Med. Chem. Commun., 2018, Advance Article
DOI: 10.1039/C7MD00158D, Review Article

Yingbin Shen, Tianyao Hao, Shiyi Ou, Churan Hu, Long Chen
Vaccines show great potential for both prophylactic and therapeutic use in infections, cancer, and other diseases

Applications and perspectives of nanomaterials in novel vaccine development

http://pubs.rsc.org/en/Content/ArticleLanding/2018/MD/C7MD00158D?utm_source=feedburner&utm_medium=feed&utm_campaign=Feed%3A+rss%2FMD+%28RSC+-+Med.+Chem.+Commun.+latest+articles%29#!divAbstract

Yingbin Shen,^a Tianyao Hao,^a Shiyi Ou,^a Churan Hu^a and Long Chen*^a

* Corresponding authors

^a Department of Food Science and Engineering, School of Science and Engineering, Jinan University, Guangzhou 510632, China
E-mail: shenybin412@gmail.com, daisyhallaiesec@gmail.com, tosy@jnu.edu.cn, hucr622@gmail.com, dexterchen@jnu.edu.cn
Fax: +86 020 852 26630
Tel: +86 138 801 32918

Abstract

Vaccines show great potential for both prophylactic and therapeutic use in infections, cancer, and other diseases. With the rapid development of bio-technologies and materials sciences, nanomaterials are playing essential roles in novel vaccine formulations and can boost antigen effectiveness by operating as delivery systems to enhance antigen processing and/or as immune-potentiating adjuvants to induce or potentiate immune responses. The effect of nanoparticles in vaccinology showed enhanced antigen stability and immunogenicity as well as targeted delivery and slow release. However, obstacles remain due to the lack of fundamental knowledge on the detailed molecular working mechanism and in vivo bio-effects of nanoparticles. This review provides a broad overview of the current improvements in nanoparticles in vaccinology. Modern nanoparticle vaccines are classified by the nanoparticles’ action based on either delivery system or immune potentiator approaches. The mechanisms of interaction of nanoparticles with the antigens and the immune system are discussed. Nanoparticle vaccines approved for use are also listed. A fundamental understanding of the in vivo bio-distribution and the fate of nanoparticles will accelerate the rational design of new nanoparticles comprising vaccines in the future.

Image result for Department of Food Science and Engineering, School of Science and Engineering, Jinan University

Department of Food Science and Engineering, School of Science and Engineering, Jinan University

//////////////nanomaterials, vaccine

A practical synthesis of 2,3-dihydro-1,5-benzothiazepines

spectroscopy, SYNTHESIS Comments Off

Dec 082017

A practical synthesis of 2,3-dihydro-1,5-benzothiazepines

Green Chem., 2017, 19,5703-5707
DOI: 10.1039/C7GC02097J, Paper

Domenico C. M. Albanese, Nicoletta Gaggero, Meng Fei
Hexafluoro-2-propanol as the solvent allows a catalyst free domino approach to 2,3-dihydro-1,5-benzothiazepines in up to 98% yield.

A practical synthesis of 2,3-dihydro-1,5-benzothiazepines

Domenico C. M. Albanese,^a Nicoletta Gaggero*^b and Meng Fei^b

*Corresponding authors

^aDepartment of Chemistry, Università degli Studi di Milano, via C. Golgi 19, Milano, Italy

^bDepartment of Pharmaceutical Sciences, Università degli Studi di Milano, via L. Mangiagalli 25, Milano, Italy
E-mail:nicoletta.gaggero@unimi.it

Domenico C. M. Albanese

University of Milan

LocationMilano, Italy

DepartmentDepartment of Chemistry

Positionassociate professor

Domenico Albanese received his Ph.D. degree in 1993 with Prof. Dario Landini working on phase transfer catalysis. After short stays at Imperial College London and the Technical University of Denmark, he gained a permanent position at the Università degli Studi di Milano, where he was appointed associate professor in 2008. His research interests include novel developments of phase-transfer catalysis, green chemistry and the development of new environmentally friendly antifouling agents.

University of Milan

image file: c4ra11206g-p2.tif

Nicoletta Gaggero

Nicoletta Gaggero received her Ph.D. degree in 1992 working on stereoselective reactions with natural proteins, enzymes and models of enzymes. After working at the Laboratoire de Chimie de Coordination du CNRS of Toulouse, she obtained a permanent position at the Università degli Studi di Milano. Her research interests cover the field of biocatalysis and asymmetric synthesis.

Abstract

2,3-Dihydro-1,5-benzothiazepines have been obtained through a domino process involving a Michael addition of 2-aminothiophenols to chalcones, followed by in situ cyclization. Up to 98% chemical yields have been obtained at room temperature under essentially neutral conditions by using hexafluoro-2-propanol as an efficient medium.

http://pubs.rsc.org/en/Content/ArticleLanding/2017/GC/C7GC02097J?utm_source=feedburner&utm_medium=feed&utm_campaign=Feed%3A+rss%2FGC+%28RSC+-+Green+Chem.+latest+articles%29#!divAbstract

2,4-Diphenyl-2,3-dihydro-1,5-benzothiazepine (4a)

Yellow solid; mp 114-116 C [lit.1 , 114-115 °C], AcOEt/PE 1:9. 1H NMR (300 MHz, CDCl3,): 3.07 (t, J = 12.6 Hz, 1 H), 3.32 (dd, J = 4.7, 13.1 Hz, 1 H), 4.99 (dd, J = 4.5, 12.0 Hz, 1 H), 7.12-7.17 (m, 1 H), 7.25-7.30 (m, 5 H), 7.44-7.51 (m, 4 H), 7.62 (d, J = 6.1 Hz, 2 H), 8.06 (d, J = 7.5 Hz, 2 H). Isolated Yield: 339 mg, 86%.

2-(4-Hydroxyphenyl)-4-phenyl-2,3-dihydro-1,5-benzothiazepine (4e)

Light brown solid; mp 131-134 °C. AcOEt/PE 40:60.

1H NMR (CDCl3, 300 MHz):  = 3.01 (t, J = 12.7 Hz, 1 H), 3.28 (dd, J = 4.8, 12.9 Hz, 1 H), 4.95 (dd, J = 4.7, 12.5 Hz, 1 H), 5.10 (bs, 1 H), 6.76 (d, J = 8.5 Hz, 2 H), 7.18-7.21 (m, 3 H), 7.35 (d, J = 8.5 Hz, 1 H), 7.46- 7.55 (m, 4 H), 7.63 (dd, J =1.5, 7.7 Hz, 1 H), 8.06 (m, 2 H).

13C NMR (CDCl3, 75 MHz): 37.99 (CH2), 60.07 (CH), 115.53 (CH), 123.08 (C), 127.40 (CH), 128.79 (CH), 131.17 (CH), 136.54 (C), 141.59 (C), 155.24 (C). IR (KBr): 1599, 2921, 3350 cm-1 .

MS (ESI): m/z= 332.24 (MH)+ .

Anal. Calcd. for C21H17NOS: C, 76.10; H, 5.17; N, 4.23, found: C, 76.21; H, 5.15; N, 4.24.

Isolated Yield: 360 mg, 87%.

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‘

“ALL FOR DRUGS” CATERS TO EDUCATION GLOBALLY, No commercial exploits are done or advertisements added by me. This is a compilation for educational purposes only. P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent

Persulfurated Coronene: A New Generation of “Sulflower”

spectroscopy, SYNTHESIS, Uncategorized Comments Off

Dec 062017

2073844-77-4

C₂₄ S_{12, 673.04}

Coroneno[1,12-cd:2,3-c‘d‘:4,5-c”d”:6,7-c”’d”’:8,9-c””d””:10,11-c””’d””’]hexakis[1,2]dithiole

A persulfurated coronene, a molecule dubbed a “sulflower” for its resemblance to a sunflower, bloomed this year. It’s the first fully sulfur-substituted polycyclic aromatic hydrocarbon and only the second member of a new class of circular heterocyclic carbon sulfide compounds, after the synthesis of octathio[8]circulene a decade ago.

Chemists hope to create other class members, including the simplest one, persulfurated benzene, for use in battery cathodes and other electronic materials.

A team led by Xinliang Feng of Dresden University of Technology and Klaus Müllen of the Max Planck Institute for Polymer Research created the sulflower (J. Am. Chem. Soc. 2017, DOI: 10.1021/jacs.6b12630).

http://pubs.acs.org/doi/abs/10.1021/jacs.6b12630

Synthesis of persulfuratedcoronene (5, PSC)

5 (82 mg) as dark red solid in 61% yield. HR-MS (HR-MALDI-TOF) m/z: Calcd. for C24S12: 671.6629; Found 671.6648 [M]+; Elem. Anal. calcd. for C24S12: C, 42.83; S, 57.17. Found: C, 42.87; S, 57.13.

Persulfurated Coronene: A New Generation of “Sulflower”

Renhao Dong^†, Martin Pfeffermann^§, Dmitry Skidin^‡, Faxing Wang^†, Yubin Fu^†, Akimitsu Narita^§, Matteo Tommasini^∥, Francesca Moresco^‡

, Gianaurelio Cuniberti^‡

, Reinhard Berger^†, Klaus Müllen^*^§

, and Xinliang Feng^*^†

^† Department of Chemistry and Food Chemistry, Center for Advancing Electronics Dresden, Technische Universität Dresden, 01062 Dresden, Germany

^§ Max-Planck-Institute for Polymer Research, Ackermannweg 10, 55128 Mainz, Germany

^‡ Institute for Materials Science, Max Bergmann Center of Biomaterials, and Center for Advancing Electronics Dresden, TU Dresden, 01069 Dresden, Germany

^∥ Dipartimento di Chimica, Materiali ed Ingegneria Chimica ‘G. Natta’, Politecnico di Milano, Piazza Leonardo da Vinci 32, 20133 Milano, Italy

J. Am. Chem. Soc., 2017, 139 (6), pp 2168–2171

DOI: 10.1021/jacs.6b12630

Publication Date (Web): January 27, 2017

*muellen@mpip-mainz.mpg.de, *xinliang.feng@tu-dresden.de

We report the first synthesis of a persulfurated polycyclic aromatic hydrocarbon (PAH) as a next-generation “sulflower.” In this novel PAH, disulfide units establish an all-sulfur periphery around a coronene core. The structure, electronic properties, and redox behavior were investigated by microscopic, spectroscopic and electrochemical methods and supported by density functional theory. The sulfur-rich character of persulfurated coronene renders it a promising cathode material for lithium–sulfur batteries, displaying a high capacity of 520 mAh g^–1 after 120 cycles at 0.6 C with a high-capacity retention of 90%

Renhao Dong

Image result for Renhao Dong DRESDEN

Research Group Leader

Renhao received his PhD in Physical Chemistry from Shandong University in 2013. Since 01/2017, he is a research group leader at the Chair for Molecular Functional Materials in TUD. His current research interest focuses on synthesis of organic 2D crystals (2D polymers/COFs/MOFs) and their applications in electronics and energy technology.

Contact

Phone: +49 – 351 / 463-40401 or -34932
Email: renhao.dong@tu-dresden.de

Prof. Xinliang Feng

Work Biography:

This is a professorship in the context of the cluster of excellence cfaed.

Xinliang Feng received his Bachelor’s degree in analytic chemistry in 2001 and Master’s degree in organic chemistry in 2004. Then he joined Prof. Klaus Müllen’s group at the Max Planck Institute for Polymer Research for PhD thesis, where he obtained his PhD degree in April 2008. In December 2007 he was appointed as a group leader at the Max-Planck Institute for Polymer Research and in 2012 he became a distinguished group leader at the Max-Planck Institute for Polymer Research.

His current scientific interests include graphene, two-dimensional nanomaterials, organic conjugated materials, and carbon-rich molecules and materials for electronic and energy-related applications. He has published more than 370 research articles which have attracted more than 25000 citations with H-index of 75.

He has been awarded several prestigious prizes such as IUPAC Prize for Young Chemists (2009), Finalist of 3rd European Young Chemist Award, European Research Council (ERC) Starting Grant Award (2012), Journal of Materials Chemistry Lectureship Award (2013), ChemComm Emerging Investigator Lectureship (2014), Highly Cited Researcher (Thomson Reuters, 2014, 2015 and 2016), Fellow of the Royal Society of Chemistry (FRSC, 2014). He is an Advisory Board Member for Advanced Materials, Journal of Materials Chemistry A, ChemNanoMat, Energy Storage Materials, Small Methods and Chemistry -An Asian Journal. He is also one of the Deputy Leaders for European communitys pilot project Graphene Flagship, Head of ESF Young Research Group “Graphene Center Dresden”, and Working Package Leader of WP Functional Foams & Coatings of GRAPHENE FLAGSHIP.

Academic Employment

12/2007-12/2012: Group Leader, Max Planck Institute for Polymer Research in Mainz, Germany
06/2010: Director of the Institute of Advanced Organic Materials, Shanghai Jiao Tong University
03/2011: Distinguished Adjunct Professorship in Shanghai Jiao Tong University, Chin
12/2012-07/2014: Distinguished Group Leader, Max Planck Institute for Polymer Research in Mainz, Germany
08/2014: W3 Chair Professor, Technische Universität Dresden, Germany

Honors and Duties

Marie Currie Fellowship (2005-2006)
Chinese Government Award for Outstanding Self-financed Students (2008)
IUPAC Prize for Young Chemists (2009)
Finalist of 3rd European Young Chemist Award (2010)
ISE (International Society of Electrochemistry) Young Investigator Award (2011)
Adjunct Professorship, China University of Geosciences (Wuhan) (2011)
Deputy Leader of one of the ten European representatives of the European community’s pilot project GRAPHENE FLAGSHIP (2012)
EU FET Young Explorer (2012)
ERC Starting Grant Award (2012)
Advisory Board Member for Advanced Materials (2013)
Journal of Materials Chemistry Lectureship Award (2013)
Advisory Board Member for Journal of Materials Chemistry A (2014)
Editorial Board Member of Chemistry – An Asian Journal (2014)
ChemComm Emerging Investigator Lectureship (2014)
Highly Cited Researcher (Thomson Reuters, 2014)
Fellow of the Royal Society of Chemistry (2014)
Highly Cited Researcher (Chemistry and Materials Science) (2015)
International Advisory Board of Energy Storage Materials (2015)
International Advisory Board of ChemNanoMat (2015)
Highly Cited Researcher (Chemistry and Materials Science, Thomson Reuters) (2016)
Head of ESF Young Research Group “Graphene Center Dresden” (2016)
Working Package Leader of WP Functional Foams & Coatings of GRAPHENE FLAGSHIP (2016)
International Advisory Board of Small Methods (2016)
Path Leader of 2.5D path within the cluster of excellence CFAED (2016)
ERC Proof-of-Concept Project Award (2017)
Small Young Innovator Award (2017)
Hamburg Science Award (2017)

Referee for:

Nature, Science, Nature Materials, Nature Nanotechnology, Nature Chemistry, Journal of the American Chemical Society, Angewandte Chemie International Edition, Nano Letters, Advanced Materials, Chemical Society Reviews, ACS Nano, Small, Chemical Communications, Chemistry of Materials, Organic Letters, Journal of the Organic Chemistry, Chemistry – A European Journal, ChemSusChem, ChemPhysChem, Macromolecular Rapid Communications, Journal of Material Chemistry, New Journal of Chemistry, Chemistry – An Asian Journal, ACS Applied Materials & Interfaces, Energy & Environmental Science, Organic Electronics and so on

Referee for research grants in NSF, US Department of Energy, ESF, ISF and Fondazione Cariparo and Fondazione CariModena.

Publications

Click to open publications list

Contact (Secretariat)

Phone: +49 351 / 463-43251
Fax: +49 351 / 463-43268
Email: sabine.strecker@tu-dresden.de

Klaus Müllen
Max-Planck-Institute for Polymer Research, Mainz, 55128, Germany

Research into energy technologies and electronic devices is strongly governed by the available materials. We introduce a synthetic route to graphenes which is based upon the cyclodehydrogenation (“graphitization”) of well-defined dendritic (3D) polyphenylene precursors. This approach is superior to physical methods of graphene formation such as chemical vapour deposition or exfoliation in terms of its (i) size and shape control, (ii) structural perfection, and (iii) processability (solution, melt, and even gas phase). The most convincing case is the synthesis of graphene nanoribbons under surface immobilization and in-situ control by scanning tunnelling microscopy.
Columnar superstructures assembled from these nanographene discs serve as charge transport channels in electronic devices. Field-effect transistors (FETs), solar cells, and sensors are described as examples.
Upon pyrolysis in confining geometries or “carbomesophases”, the above carbon-rich 2D- and 3D- macromolecules transform into unprecedented carbon materials and their carbon-metal nanocomposites. Exciting applications are shown for energy technologies such as battery cells and fuel cells. In the latter case, nitrogen-containing graphenes serve as catalysts for oxygen reduction whose efficiency is superior to that of platinum.

Müllen, K., Rabe, J.R., Acc. Chem. Res. 2008, 41, (4), 511-520;
Wang, X., Zhi, L., Müllen, K. Nano. Lett. 2008, 8, 323-327;
Feng, X.; Chandrasekhar, N.; Su, H. B.; Müllen, K., Nano. Lett. 2008, 8, 4259.;
Pang, S.; Tsao, H. N.; Feng, X.; Müllen, K., Adv. Mater. 2009, 31, 3488;
Feng, X., Marcon, V., Pisula, W., Hansen, M.R., Kirkpatrick, I., Müllen, K., Nature Mater. 2009, 8, 421;
Cai, J., Ruffieux, P., Jaafar, R., Bieri, M., Braun, T., Blankenburg, S., Muoth, M., Seitsonen, A. P., Saleh, M., Feng, X., Müllen, K., Fasel, R., Nature 2010, 466, 470-473;
Yang, S., Feng, X., Zhi, L., Cao, Q., Maier, J., Müllen, K., Adv. Mater. 2010, 22, 838; Liu, R., Wu, D., Feng, X., Müllen, K., Angew. Chem. Int. Ed. 2010, 49, 2565;
Käfer, D., Bashir, A., Dou, X., Witte, G., Müllen, K., Wöll, C., Adv. Mater. 2010, 22, 384;
Diez-Perez, I., Li, Z., Hihath, J., Li, J., Zhang, C., X., Zang, L., Dai, Y., Heng, X., Müllen, K., Tao, N. J. Nature Commun. 2010, DOI: 10.1038.

Prof. Dr. Klaus Müllen
joined the Max-Planck-Society in 1989 as one of the directors of the Max-Planck Institute for Polymer Research. He obtained a Diplom-Chemiker degree at the University of Cologne in 1969 after work with Professor E. Vogel. His Ph.D. degree was granted by the University of Basel, Switzerland, in 1972 where he undertook research with Professor F. Gerson on twisted pi-systems and EPR spectroscopic properties of the corresponding radical anions. In 1972 he joined the group of Professor J.F.M. Oth at the Swiss Federal Institute of Technology in Zürich where he worked in the field of dynamic NMR spectroscopy and electrochemistry. He received his habilitation from the ETH Zürich in 1977 and was appointed Privatdozent. In 1979 he became a Professor in the Department of Organic Chemistry, University of Cologne, and accepted an offer of a chair in Organic Chemistry at the University of Mainz in 1983. He received a call to the University of Göttingen in 1988.

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http://pubs.acs.org/doi/abs/10.1021/jacs.6b12630

https://cen.acs.org/articles/95/i49/molecules-of-the-year-2017.html?utm_source=Twitter&utm_medium=Social&utm_campaign=CEN&hootPostID=ea1deb5464b6231122901a3321f4ff5e

“ALL FOR DRUGS” CATERS TO EDUCATION GLOBALLY, No commercial exploits are done or advertisements added by me. This is a compilation for educational purposes only. P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent

A derivatisation agent selection guide frequently applied in analytical chemistry and related disciplines.

Uncategorized Comments Off

Dec 032017

A derivatisation agent selection guide

Green Chem., 2017, Advance Article
DOI: 10.1039/C7GC03108D, Paper

Open Access

This article is licensed under a Creative Commons Attribution-NonCommercial 3.0 Unported Licence.

Marek Tobiszewski, Jacek Namiesnik, Francisco Pena-Pereira
The study reported herein is aimed at the greenness assessment of 267 derivatisation agents that are frequently applied in analytical chemistry and related disciplines.

A derivatisation agent selection guide

Marek Tobiszewski,^a Jacek Namieśnik^a and Francisco Pena-Pereira*^b

*Corresponding authors

^aDepartment of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology (GUT), 11/12 G. Narutowicza St., 80-233 Gdańsk, Poland

^bDepartment of Analytical and Food Chemistry, Faculty of Chemistry, University of Vigo, Campus As Lagoas – Marcosende s/n, 36310 Vigo, Spain
E-mail:fjpena@uvigo.es

Abstract

The study reported herein is aimed at the greenness assessment of 267 derivatisation agents that are frequently applied in analytical chemistry and related disciplines. Multicriteria decision analysis allowed obtaining three rankings of derivatisation agents applied in liquid chromatography, gas chromatography and chiral analysis. The criteria of assessment included the safety information obtained from material safety data sheets and physicochemical and environmental parameters predicted with relevant models. As for some of the agents predicted data were not available, these agents were assessed with a smaller number of criteria, within the ranking of low confidence. The results of the study will help to apply greener derivatisation agents, wherever the green chemistry principle of avoiding derivatisation cannot be fulfilled.

The present study provides an assessment, in terms of greenness, of 267 LC, GC and chiral derivatisation agents typically used in analytical chemistry and related fields. The preference rankings were performed for each group of derivatisation agents by means of MCDA according to the best relevant criteria that are available. In all three cases fine rankings were obtained for high and low confidence assumptions. For more informative assessment, it would be beneficial to include toxicological endpoints and more information about environmental persistence among assessment criteria. Incorporating valuable greenness indicators of synthesis processes such as carbon footprint or energy needs during production of each chemical as assessment criteria would be worthwhile. Unfortunately, these values are not easily available in the literature for a satisfactory number of derivatisation agents. Furthermore, recovery of derivatisation agents is another important issue that influences the greenness of derivatisation reactions, so its inclusion as assessment criterion would also be desirable. However, it is dependent on reaction specific conditions – not only the kind of derivatisation agent matters, but also analytes to be determined and solvents employed. The greenness of derivatisation agents is very rarely considered during analytical method development. The main criteria for selection of derivatisation agents are their rapidity and efficiency, but greenness should be also considered. This study allows selecting less problematic derivatisation agents for analytical method development while some clues can also be deduced for other than analytical applications.

http://pubs.rsc.org/en/Content/ArticleLanding/2017/GC/C7GC03108D?utm_source=feedburner&utm_medium=feed&utm_campaign=Feed%3A+rss%2FGC+%28RSC+-+Green+Chem.+latest+articles%29#!divAbstract

Image result for Gdańsk University of Technology

Gdańsk University of Technology

Image result for Marek Tobiszewski gdansk

Marek Tobiszewski,

Department of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology (GUT), 11/12 G. Narutowicza St., 80-233 Gdańsk, Poland

Marek Tobiszewski

Gdansk University of Technolog… , Gdańsk · Department of Analytical Chemistry

Jacek Namieśnik

Gdansk University of Technolog… , Gdańsk · Department of Analytical Chemistry

Francisco Javier Pena-Pereira

PhD

PostDoc Position

University of Vigo , Vigo · Department of Analytical and Food Chemistry

Research experience

Apr 2013–present

Universidade de Vigo · Department of Analytical and Food Chemistry

Spain · Vigo
Apr 2011–Mar 2013

University of Aveiro · Centre for Environmental and Marine Studies (CESAM)

Portugal · Aveiro
Jun 2005–Apr 2011

Universidade de Vigo · Department of Analytical and Food Chemistry

Spain · Vigo

Faculty of Chemistry, University of Vigo

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Catalytic C-H amination at its limits: challenges and solutions

organic chemistry, Uncategorized Comments Off

Nov 232017

Catalytic C-H amination at its limits: challenges and solutions

Org. Chem. Front., 2017, 4,2500-2521
DOI: 10.1039/C7QO00547D, Review Article

Damien Hazelard, Pierre-Antoine Nocquet, Philippe Compain
Pushing C-H amination to its limits fosters innovative synthetic solutions and offers a deeper understanding of the reaction mechanism and scope.

Catalytic C–H amination at its limits: challenges and solutions

Damien Hazelard,^a Pierre-Antoine Nocquet^a and Philippe Compain*^a

*Corresponding authors

^aLaboratoire de Synthèse Organique et Molécules Bioactives (SYBIO), Université de Strasbourg/CNRS (UMR 7509), Ecole Européenne de Chimie, Polymères et Matériaux (ECPM), 25 rue Becquerel, 67087 Strasbourg Cedex 2, France
E-mail: philippe.compain@unistra.fr

Abstract

Catalytic C–H amination reactions enable direct functionalization of non-activated C(sp³)–H bonds with high levels of regio-, chemo- and stereoselectivity. As a powerful tool to unlock the potential of inert C–H bonds, C–H amination chemistry has been applied to the preparation of synthetically challenging targets since major simplification of synthetic sequences are expected from this approach. Pushing C–H amination to its limits has led to a deeper understanding of the reaction mechanism and scope. In this review, we present a description of the specific challenges facing catalytic C–H amination in the synthesis of natural products and related compounds, as well as innovative tactics created to overcome them. By identifying and discussing the major insights gained and strategies designed, we hope that this review will stimulate further progress in C–H amination chemistry and beyond.

Conclusion Since the seminal works of Du Bois in the early 2000s, the pace of discovery in the field of metal-catalysed C–H amination has been breath-taking. Not surprisingly, this synthetic tool has been applied to the total synthesis of many compounds of interest, given the high prevalence of the amino group in natural products and synthetic pharmaceuticals.67 Chemist’s confidence in the high potential of the C–H amination methodology to unlock inert C–H bonds has been demonstrated by its application to more and more challenging substrates. This has been a powerful drive for progress in the field. New valuable insights have been gained allowing, for example, a better regiochemical control via stereoelectronic and/or conformational effects. Innovative strategies have been discovered to direct the insertion event in substrates bearing a large degree of attendant functionality. Solutions have spanned from the elegant exploitation of kinetic isotope effects to the tactical use of protecting groups with different sizes or electronic characteristics. Systematic exploration of different catalytic systems has been also performed leading to the opening of new possibilities in C–H amination technology. Manganese-based catalysts have thus given rise to nitrenoids that overcome the low reactivity of primary aliphatic C–H bonds without interfering with weaker secondary/tertiary C–H bonds. Despite these impressive achievements, much remains to be done. Counterintuitive selectivity and unexplained reactivity should serve as a reminder that further studies are highly needed to understand in depth catalytic C–H amination chemistry. Many challenges remain on the way, from basic to applied research. A clear mechanistic view based on definitive evidence concerning the details of the C–N bond forming process would undoubtedly facilitate the rational design of efficient catalytic systems leading to higher regio-, chemio- and stereoselectivity. In particular, the quest for site-selective C–H amination through catalyst control has to be pursued.10d,e In this context, the development of efficient intermolecular C–H amination process still represents a major challenge and upcoming advancements are expected to increase the impact of this technology in organic synthesis. Future progress made in the field of catalytic C–H amination chemistry might also lead to industrial-scale applications in the next decade. It is likely that total synthesis of synthetically challenging targets related to natural products will continue to be a powerful driving force towards this goal.

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“ALL FOR DRUGS” CATERS TO EDUCATION GLOBALLY, No commercial exploits are done or advertisements added by me. This is a compilation for educational purposes only. P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent

amcrasto@gmail.com

Highly active, separable and recyclable bipyridine iridium catalysts for C–H borylation reactions

spectroscopy, SYNTHESIS, Uncategorized Comments Off

Nov 212017

Graphical abstract: Highly active, separable and recyclable bipyridine iridium catalysts for C–H borylation reactions

Highly active, separable and recyclable bipyridine iridium catalysts for C–H borylation reactions

Hind Mamlouk,^a Jakkrit Suriboot,^b Praveen Kumar Manyam,^a Ahmed AlYazidi,^a David E. Bergbreiter*^b and Sherzod T. Madrahimov*^a

*Corresponding authors

^aDepartment of Chemistry, Texas A&M University at Qatar, P.O. Box 23874, Doha, Qatar
E-mail: sherzod.madrahimov@qatar.tamu.edu

^bDepartment of Chemistry, Texas A&M University, College Station, USA
E-mail: bergbreiter@tamu.edu

Abstract

Iridium complexes generated from Ir(I) precursors and PIB oligomer functionalized bpy ligands efficiently catalyzed the reactions of arenes with bis(pinacolato)diboron under mild conditions to produce a variety of arylboronate compounds. The activity of this PIB bound homogeneous catalyst is similar to that of an original non-recyclable catalyst which allows it to be used under milder conditions than other reported recyclable catalysts. This oligomer-supported Ir catalyst was successfully recovered through biphasic extraction and reused for eight cycles without a loss of activity. Biphasic separation after the initial use of the catalyst led to an insignificant amount of iridium leaching from the catalyst to the product, and no iridium leaching from the catalyst was observed in the subsequent recycling runs. Arylboronate products obtained after extraction are sufficiently pure as observed by ¹H and ¹³C-NMR spectroscopy that they do not require further purification.

Hind MAMLOUK, PhD

R&D in Organic Materials Chemistry Looking for a New Challenge

3-Chloro-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)anisole (5). Transparent oil. Yield: 87%.

1H NMR (600 MHz, CDCl3) δ 7.37 (s, 1H), 7.22 – 7.16 (m, 1H), 6.99 (s, 1H), 3.82 (s, 3H), 1.34 (s, 12H);

13C NMR (101 MHz, CDCl3) δ 159.88, 134.57, 126.84, 117.71, 117.43, 84.15, 55.52, 24.82.

GCMS: RT=14.55 min, M+ = 268.1 vs MW= 268.54 g.mol-1 .

Sherzod Madrahimov

Asst. Prof.

Texas A&M University at Qa… , Doha · Science

Research experience

Aug 2015–present

Asst. Prof.

Texas A&M University at Qatar · Chemistry

Qatar · Doha
Jul 2012–Jul 2015

PostDoc Position

Northwestern University · Department of Chemistry

United States · Evanston
Aug 2007–Jul 2012

Graduate student

University of Illinois, Urbana-Champaign · Department of Chemistry

United States · Urbana

Texas A&M University at Qatar

David Bergbreiter
Professor

Contact

Department of Chemistry
Texas A&M University
College Station, TX 77843-3255

P: 979-845-3437
F: 979-845-4719
bergbreiter@chem.tamu.edu

Current Activities

Our group explores new chemistry related to catalysis and polymer functionalization using the tools and precepts of synthetic organic chemistry to prepare functional oligomers or polymers that in turn are used to either effect catalysis in a greener, more environmentally benign way or to more efficiently functionalize polymers. Often this involves creatively combining the physiochemical properties of a polymer with the reactivity of a low molecular weight compound to form new materials with new functions. These green chemistry projects involve undamental research both in synthesis and catalysis but has practical aspects because of its relevance to practical problems.

A common theme in our catalysis studies is exploring how soluble polymers can facilitate homogeneous catalysis. Homogeneous catalysts are ubiquitously used to prepare polymers, chemical intermediates, basic chemicals and pharmaceuticals. Such catalysts often use expensive or precious metals or expensive ligands or are used at relatively high catalyst loadings. The products often contain traces of these catalysts or ligands – traces that are undesirable for esthetic reasons or because of the potential toxicity of these impurities. Both the cost of these catalysts of these issues require catalyst/product separation – separations that often are inefficient and lead to chemical waste. These processes also use volatile organic solvents – solvents that have to be recovered and separated. Projects underway in our lab explore how soluble polymers can address each of these problems. Examples of past schemes that achieve this goal in a general way as highlighted in the Figure below.

We also use functional polymers to modify existing polymers. Ongoing projects involve molecular design of additives that can more efficiently modify polymers’ physical properties. We also use functional polymers in covalent layer-by-layer assembly to surface polymers’ surface chemistry. An example of this work is our use of ‘smart’ polymers that reversibly change from being water soluble cold to being insoluble and hydrophobic on heating. Such polymers’ have been used by us to prepare ‘smart’ catalysts, ‘smart’ surfaces and membranes, and to probe fundamental chemistry underlying temperature and salt-dependent protein solvation.

Jakkrit Suriboot

Research Assistant at Texas A&M University

Image result for Praveen Kumar Manyam TEXAS

Dr. Praveen Kumar

Title: Research Assistant Professor

Education: M.S., I.I.T. Roorkee
Ph.D., Panjab University Chandigarh (2008)
Visiting Fellow (w/ Prof. G. G. Balint-Kurti), Bristol University, UK
Postdoctoral Research Associate (w/ Prof. Svetlana Malinovskaya), Stevens Institute of Technology, Hoboken, NJ
Senior Postdoctoral Research Associate (w/ Prof. Seogjoo Jang), Queens College of CUNY, NY

Office: Chemistry 010

Phone: 806-742-3124

Email: praveen.kumar@ttu.edu

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“ALL FOR DRUGS” CATERS TO EDUCATION GLOBALLY, No commercial exploits are done or advertisements added by me. This is a compilation for educational purposes only. P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent

amcrasto@gmail.com

Biovis PSA2000 Automated Particle Size Analysis System (The 21 CFR Part 11 compliance module )

Uncategorized Comments Off

Nov 122017

Inline images 1

Biovis PSA2000

Automated Particle Size Analysis System

Biovis PSA 2000 system designed to provide particle size and shape analysis with more than 70 measurements on size shape and color makes it a unique solution for R&D and QC applications in Pharmaceutical, Food processing, Paint , Ink Coating and many other applications. The 21 CFR Part 11 compliance module make it more preferred for the Manufacturing plants working under USFDA guidelines. Report available on request, or download link available below, it is as per the regulatory requirements.

For R&D the non FDA version of the software can provide huge amount of data which can be mined to help find more information about the particulate matter based on its size and shape thereby improve the Drug delivery, Process Engineering , process development etc…

Biovis PSA2000 is an automated particle size analysis system for comprehensive investigation of different types of dry or wet particulate matter such as fibres, emulsions, crystals, powders, spray droplets, or suspensions, etc.

– Rapid automated analysis of thousands of individual particles

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– Custom built analysis routines to handle specific sample types

– Detect and classify particle types on the basis of size, shape, color

– Professional Analysis Report generation

The Biovis PSA 2000 system with Biovis Particle Plus Ver 5.3 has the following features

Reports with D10, D50, D90 values.
Number and Volume distribution charts
Administrator driven Login Policies.
Powerful macros/methods for automatic detection of different types of samples to achieve repeatable results with different users for same samples.
Micro Image documentation with Electronic Signature as per 21 CFR Part II compliance guidelines.
Complete audit trail to trace every action in each experiment.

Departments that can benefit from Biovis PSA 2000 system are

Process development/ Process Engineering
Quality Control ( Finished Material/ Inward Raw Material)
Performance of finished product ( Aspect ratio /roundness factor helps better design of final product)
Research and Development

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Imaging Solutions

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Image Analysis Software are used in the field of Pathology, MicroBiology, research & quality control of Medicine, Forensic sciences, etc.
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is perfectly suited for these applications and provides numerous functions for enhancement of Image and then obtaining morphometric, densitometry and stereological measurements.

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The

Biovis PSM

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Biovis Materials Plus

is aimed at providing solutions for these Material analysis requirements.

Naveen Hegde

Regards

Naveen Hegde

Expert Vision Labs

H202, Ranjit Studio,

DP Road, Dadar East,

Mumbai 400014

India.

Tel:+91 22 6637 2739 / +91 22 6637 1470

Mobile: +91 93240 51848

Fax : +91 22 6637 2739

Website : www.expertvisionlabs.com

email : nhegde@expertvisionlabs.com

Expert Vision Labs

Expert Vision Labs has pioneered Image Analysis Technology in India and has focus into developing, a flexible line of highly cost effective and quality software driven products for Research and Industrial customers in India and across the globe.
Established in 1995, Expert Vision Labs has strived to specialize in providing complete solutions for computer based imaging and vision related applications. Have developed the

Biovis

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Report available on request, or download here is as per the regulatory requirements.
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