专利号:US-2015239909-A1 优先权日:2012-11-23 标 题 :Process for the preparation of (1s,4s,5s)-4-bromo-6-oxabicyclo[3.2.1]octan-7-one 发明人:NAKAMURA YOSHITAKA; MUKESH Kumar Madhra; INAMDAR MURAD ISMAIL 权利人:DAIICHI SANKYO CO LTD 摘要:The present invention relates to an improved and industrially advantageous process for the preparation of (1S, 4S, 5S)-4-bromo-6-oxabicyclo[3.2.1]octan-7-one represented by the following formula (1) n n n n n n n n n n which is a key intermediate in the synthesis of edoxaban, a compound that exhibits on inhibitory effect on activated blood coagulation factor X (also referred to as activated factor X or FXa), and is useful as a preventive and/or therapeutic drug for thrombotic diseases. The process includes reacting (1S)-cyclohex-3-ene-1-carboxylic acid of formula (II) with a brominating agent selected from the group consisting of N-bromosuccinimide or 1,3-dibromo-5, 5-dimethylhydantoin in the presence of a base selected from calcium oxide or calcium hydroxide in a solvent selected from the group comprising of dicholoromethane, toluene, tetrahydrofuran, ethyl acetate, hexanes, cyclopentyl methyl ether (CPME) or a misture thereof to get (1S, 4S 5S)-4-bromo-6-oxabicyclo[3.2.1]octan-y-one of formula (1)
专利号:US-9809546-B2 优先权日:2016-03-14 标 题 :Process for producing diamine derivative 发明人:LU TZU-CHIANG; CHEN CHIEN-YI; CHENG CHING-SHUEN; MAI CHIN-CHENG 权利人:CHUNGHWA CHEMICAL SYNTHESIS & BIOTECH CO LTD; CHUNGWHA CHEMICAL SYNTHESIS & BIOTECH CO LTD 摘要:The present invention provides a low-toxic and high-recovery industrial process for synthesizing an optically active diamine derivative represented by formula (D), the process comprising the steps of: (a) mixing a compound represented by formula (A) and a compound represented by formula (C) in organic solvents and secondary amine; (b) reaction under heating; (c) cooling and adding water to the mixed solution, allowing it to crystallize to obtain the compound represented by formula (D).
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合成参考文献
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