115581-36-7Relevant articles and documents
Preparation method of 2-chloro-5-methylthiopyrimidine
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Paragraph 0042-0044; 0049-0053; 0057-0059; 0063-0067; 0071, (2021/04/21)
The invention discloses a preparation method of 2-chloro-5-methylthiopyrimidine, wherein the preparation method comprises the following steps: firstly, dissolving 5-bromo-2-chloropyrimidine, namely a compound 1, in dimethylformamide, adding sodium methyl mercaptide, and reacting to obtain 2,5-dimethylthiopyrimidine, namely a compound 2; adding 2,5-dimethylthiopyrimidine, namely the compound 2, into a hydrochloric acid aqueous solution, and then reacting and refluxing to obtain 2-hydroxy-5-methylthiopyrimidine, namely a compound 3; adding 2-hydroxy-5-methylthiopyrimidine, namely the compound 3, into POCl3, dropwise adding N,N-dimethylaniline, and reacting to obtain 2-chloro-5-methylthiopyrimidine, namely a final compound. The technical problem that no suitable industrial synthesis method is available at present is mainly solved. The method provided by the invention can reduce the production cost for preparing 2-chloro-5-methylthiopyrimidine, the total yield is significantly improved to 89%, and the method is suitable for kilogram-level scale-up production, the raw materials are easy to obtain, the operation is convenient, the reaction is easy to control, and column chromatography purification is not needed.
SUCCINATE AND FUMARATE ACID ADDITION SALTS OF PIPERAZINE DERIVATIVES USEFUL AS GLYCOSIDASE INHIBITORS
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Page/Page column 33, (2020/03/15)
The invention relates to succinic acid addition salts or fumaric acid addition salts of piperazine derivatives of formula (I), as well as solid forms, such as polymorphic forms, thereof, which are useful as pharmaceutical ingredients and in particular as
HETEROCYCLIC AMIDES AS KINASE INHIBITORS
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Page/Page column 72, (2019/07/17)
Disclosed are compounds having the formula (I) wherein R1, R2, and R3 are as defined herein, and methods of making and using the same.