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Asian Journal of Research in Chemistry
Year : 2018, Volume : 11, Issue : 3
First page : ( 539) Last page : ( 544)
Print ISSN : 0974-4169. Online ISSN : 0974-4150.
Article DOI : 10.5958/0974-4150.2018.00096.2

Isolation and structure characterization of related impurity in olanzapine key starting material by LC/ESI-MS and NMR

Narkedimilli Jagadeesh1,2,*, Vavilala Vishweshwar1, Mohanty Sandeep1, Manvalan Saravanan1, Anireddy Jayashree2

1Dr. Reddy's Laboratories Limited, API Plant, Bollaram-III, Plot No 116, IDA Bollaram, Medak District, Hyderabad, 502325, Telangana, India

2Centre for Chemical Sciences and Technology, Institute of Science and Technology, Jawaharlal Nehru Technological University, Hyderabad, Kukatpally, Hyderabad, 500085, Telangana, India

*Corresponding Author E-mail: jagadeeshn@drreddys.com

Online published on 21 August, 2018.

Abstract

Olanzapine key starting material, 5-methyl-2-((2-nitrophenyl)amino)thiophene-3-carbonitrile (3), is a key starting material of Olanzapine. During the impurity profile study an unknown peak was detected by HPLC and MS methods. Identification, isolation and structural characterization in olanzapine key starting material is described in this article. The impurity was isolated by preparative HPLC, Based on the complete spectral analysis, MS, 1D NMR (1H and 13C) and 2D NMR (COSY, HSQC and HMBC) the chemical structure of unknown impurity was characterized as 2-(bis(2-nitrophenyl)amino)-5-methylthiophene-3-carbonitrile.

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Keywords

Liquid chromatography-mass spectrometry, NMR, Characterization, impurity profile, Olanzapine.

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