Preparation method of linagliptin

The invention discloses a preparation method of linagliptin. The preparation method comprises putting t-butyloxycarbonyl-linagliptin (g) into a methanol aqueous solution and carrying out stirring so that the solution undergoes a reaction along with heating reflux in an inert atmosphere at a temperat...

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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 preparation method of linagliptin. The preparation method comprises putting t-butyloxycarbonyl-linagliptin (g) into a methanol aqueous solution and carrying out stirring so that the solution undergoes a reaction along with heating reflux in an inert atmosphere at a temperature of 25-50 DEG C for 3-12h, wherein a weight ratio of the t-butyloxycarbonyl-linagliptin (g) to the methanol aqueous solution is 100: (400-550). The preparation method carries out Boc protection base removal in a methanol aqueous solution in an inert gas protective atmosphere, is free of expensive trifluoroacetic acid-DCM in a Boc protection base removal reaction, only utilizes a cheap methanol-water system and has simple after-treatment processes. A trifluoroacetic acid-DCM system reaction produces more impurities and needs a very complex post-treatment purifying process. The preparation method prevents strong acid-produced intermediate (g) impurities and linagliptin amide bond fracture impurities. 本发明公开了种利格列汀的制
Bibliography:Application Number: CN20161189178