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DR ANTHONY MELVIN CRASTO, WORLDDRUGTRACKER

Continuous Flow Doebner–Miller Reaction and Isolation Using Continuous Stirred Tank Reactors

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Aug 312016
 

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Continuous flow Doebner–Miller synthesis of different quinaldines from respective anilines is demonstrated using sulfuric acid as a homogeneous catalyst. The extent of reaction was monitored for various parameters, namely, temperature, residence time, mole ratio of sulfuric acid to substrate, mole ratio of crotonaldehyde to substrate, and so forth. Continuous stirred reactors in series were used as a preferred configuration for this rection that generates byproduct in the form of sticky solid material. The approach has been extended for six different anilines, and the results are compared with batch reactions. Continuous stirred reactors in series with distributed dosing of crotonaldehyde facilitated a continuous flow reaction with lower byproduct formation, increased yields, and continuous workup and is a scalable approach.

 

Continuous Flow Doebner–Miller Reaction and Isolation Using Continuous Stirred Tank Reactors

Chem. Eng. & Process Dev. Division, CSIR-National Chemical Laboratory, Dr. Homi Bhabha Road, Pashan, Pune 411 008, India
Organic Chemistry Division, CSIR-National Chemical Laboratory, Dr. Homi Bhabha Road, Pashan, Pune 411 008, India
Org. Process Res. Dev., Article ASAP
DOI: 10.1021/acs.oprd.6b00179
Publication Date (Web): August 22, 2016
Copyright © 2016 American Chemical Society
*E-mail: aa.kulkarni@ncl.res.in. Fax: +91-20-25902621.
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Mr. Maruti Yadav
Project Assistant
M.Sc. Organic Chemistry, Pune University, 2013
Process Development of API production in continuous flow
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Dr. Amol A. Kulkarni

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Dr. Amol A. Kulkarni is a Scientist in the Chemical Engineering Division at the National Chemical Laboratory. He did his B. Chem. Eng. (1998), M. Chem. Eng (2000) and Ph.D. in chemical engineering (2003) all from the University Dept. of Chem. Technology (UDCT, Mumbai). In 2004 he worked at the Max Planck Institute-Magdeburg (Germany) as a Alexander von Humboldt Research Fellow. At NCL he is driving a research program on the design of microreactors and exploring their applications for continuous syntheses including of nanoparticles. He has been awarded with the Max-Planck-Visiting Fellowship from the Max-Planck-Society, Munich for 2008-2011. His research areas include: (i) design and applications of microreactors, (ii) design of multiphase reactors, (iii) experimental and computational fluid dynamics, and (iv) nonlinear dynamics of coupled systems. He is an active member of Initiative for Research and Innovation in Science (IRIS) supported by Intel’s Education Initiative to organize National Science Fair and popularize science in India.

Research areas

  • Multiphase reactors and Microreactors
  • Process Development and Scale-up
  • Process Intensification & MAGIC Processes
  • Industrial Flow Processes

Contact

  • Dr. Amol A. Kulkarni
    Scientist
    Office: 529, PP-1 Building, CEPD
    National Chemical Laboratory
    Dr. Homi Bhabha Road
    Pune 411008, India
    Phone  +91 20 2590 2153
    Fax +91 20 2590 2621
    E-mail aa.kulkarni@ncl.res.in

///////////Continuous Flow,  Doebner–Miller Reaction, Isolation, Continuous Stirred Tank Reactors, chemical engeineering, process, Amol A. Kulkarni, ncl, pune

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Sep 252013
 

File:Zolmitriptan.svg

ZOLMITRIPTAN

 A paper from Emcure

Four isomeric unknown impurities ranging from 0.08-0.12% were found in the purified sample of Zolmitriptan during the batch analysis by gradient reverse phase ultra performance liquid chromatography (UPLC) and their molecular weights determined by liquid chromatography mass spectroscopy (LC-MS) analysis. Subsequently, all the four impurities were isolated by flash chromatography followed by semi-preparative HPLC and characterized by 1H NMR, 13C NMR, 1H-1H COSY, HMBC, HSQC, MS spectroscopy and HPLC. The structures for these four impurities were assigned to be following
Isomeric Impurity-1: 4-((3-(2-(dimethylamino)ethyl)-4-(2-((oxazolidin-4-yl)methyl)phenyl)-1H-indol-5-yl)methyl) oxazolidin-2-one,
Isomeric Impurity-2: 4-((3-(2-(dimethylamino)ethyl)-2-(4-((oxazolidin-4-yl)methyl)phenyl)-1H-indol-5-yl)methyl) oxazolidin-2-one-,
Isomeric Impurity-3: 4-((3-(2-(dimethylamino)ethyl)-7-(4-((oxazolidin-4-yl)methyl)phenyl)-1H-indol-5-yl)methyl) oxazolidin-2-one,
Isomeric Impurity-4: 4-((3-(2-(dimethylamino)ethyl)-6-(4-((oxazolidin-4-yl)methyl)phenyl)-1H-indol-5-yl)methyl) oxazolidin-2-one
Isolation and characterization of impurities has helped us in improving the purity of API by removing these impurities using crystallization.

READ ALL THIS AT

http://www.omicsonline.org/isolation-and-structural-elucidation-of-novel-isomeric-process-related-impurities-of-zolmitriptan-2155-9872.1000165.php?aid=13012#

Neelakandan K
API Research Centre
Emcure Pharmaceutical Limited
Hinjawadi, Pune, 411057, India
Fax: +91 20 39821445
E-mail: Neelakandan.K@emcure.co.in

Volume 4, Issue 2
Research Article:  J Anal Bioanal Tech 2013, 4:165
doi: 10.4172/2155-9872.1000165
Isolation and Structural Elucidation of Novel Isomeric Process Related Impurities of Zolmitriptan
Neelakandan K, Chaudhari Ashok, Manikandan H, Santosha N, Prabhakaran B and Mukund Gurjar
Citation: Neelakandan K, Ashok C, Manikandan H, Santosha N, Prabhakaran B, et al. (2013) Isolation and Structural Elucidation of Novel Isomeric Process Related Impurities of Zolmitriptan. J Anal Bioanal Tech 4:165. doi: 10.4172/2155-9872.1000165

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Mukund Keshao Gurjar

Dr. Mukund Gurjar is an Executive Director and Chief Scientific Officer (Research and Development) of this Company(Emcure). He is a graduate, a post graduate and Ph.D. in Chemistry from the Nagpur University. He also holds a second Ph. D. degree in Chemistry from the London University, United Kingdom as well as a post doctoral fellowship from Toronto, Canada. Prior to joining our Company, he was the deputy director of the National Chemical Laboratory, Pune where he spent 25 years spearheading innovative and advance research in Organic Chemistry. He has over 32 years of experience in pharmaceutical sciences and is a fellow at various national and international academies. He is a member of the editorial board of the prestigious journal Organic Process Research & Development published by the American Chemical Society. For his contributions to synthetic organic chemistry involving both basic and applied research, he has been felicitated with various awards. A large number of students have obtained Ph.Ds under the supervision of Dr. Gurjar and has published more than 200 papers in various international journals. He has been associated with our Company since 2001 and also became a member of the Board in the same year.

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