Synthesis method of linagliptin intermediate

The invention discloses a synthesis method of a linagliptin intermediate. The synthesis method comprises adding 1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butyne-1-yl)-8-bromoxanthine (e), (R)-3-Boc-aminopiperidine (f), potassium carbonate and acetonitrile into a reactor, carrying out uniform...

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Bibliographic Details
Main Authors Ji Liping, Zhang Lihua, Zhao Hongwei, Wang Jieting, Sheng Li, Cui Yujie, Ma Zheng, Wang Yanfeng
Format Patent
LanguageChinese
English
Published 31.08.2016
Subjects
CHEMISTRY
HETEROCYCLIC COMPOUNDS
METALLURGY
ORGANIC CHEMISTRY
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Summary:The invention discloses a synthesis method of a linagliptin intermediate. The synthesis method comprises adding 1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butyne-1-yl)-8-bromoxanthine (e), (R)-3-Boc-aminopiperidine (f), potassium carbonate and acetonitrile into a reactor, carrying out uniform mixing and carrying out a reaction process under the conditions of heating reflux, a reaction temperature of 80-85 DEG C and reaction time of 24-48h, wherein a mole ratio of 1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butyne-1-yl)-8-bromoxanthine (e), (R)-3-Boc-aminopiperidine (f) to potassium carbonate is 1: (1.2-1.6): (3-7) and a ratio of 1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butyne-1-yl)-8-bromoxanthine (e) to acetonitrile is 100: (400-1000)g/ml. The synthesis method of the linagliptin intermediate (g) prevents generation of debromination impurities (i), is simple and easy in a post-treatment step and solves the problem that the intermediate is not easily separated from a solvent and is diffic
Bibliography:Application Number: CN20161189177