210963-78-3Relevant academic research and scientific papers
Preparation method of betrexiban intermediate compound
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Paragraph 0053-0054; 0056-0057, (2022/02/24)
The present invention belongs to the field of drug synthesis technology, specifically relates to a method for preparing a betroxiban intermediate, the present invention prepares a method of preparing a betroxiban intermediate comprising: dissolving compound II in an organic solvent A, temperature-controlled drops plus tert-butyl dimethylsilane, drip bi, insulation reaction, TLC detection, reaction completed, dropwise addition of dimethylamino lithium solution to the reaction solution, dropwise addition, continue insulation reaction, TLC detection, reaction completion, adding ethyl acetate dilution, adding saturated ammonium chloride solution to the reaction solution wash, The organic phase is dried with anhydrous sodium sulfate, concentrated to dry under reduced pressure to obtain compound III; to provide a new method of using p-cyanobenzoic acid as raw material, using silanization reagents to protect the hydroxyl group, and obtaining a key intermediate of betroxiban, which has fewer synthetic route steps, high yield and high purity.
Preparation method of beta-caraban
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, (2021/11/10)
The preparation method comprises the following steps: in liquid dimethylamine, a compound of the structural formula II or a salt thereof and MN (CH). 3 )2 The dimethylamine solution in the structural formula I is reacted to obtain the fritilth. M represents Li or MgX; and M is Li or Na. Wherein X is selected from one of Cl, Br and I. The preparation method disclosed by the invention is high in yield and high in product purity, can substantially avoid generation of single methyl ammonia impurities and dechlorination impurities, and greatly simplifies the subsequent refining process. In addition, the preparation method is single in solvent, the use of the mixed solvent is avoided, the later-stage solvent recovery is convenient, and the three wastes can be reduced.
