CAS: 900186-72-3; (3R,3As,4S,4As,7R,9Ar)-3-Methyl-7-Nitro-1-Oxo-N,N-Diphenyl-1,3,3A,4,4A,5,6,7,8,9A-Decahydronaphtho[2,3-C]Furan-4-Carboxamide

在 三乙胺体系中,用 乙醇,异丙醇,甲苯 作为反应溶剂,以1.28 Kg的收率获得产物沃拉帕沙
参考文献:一种沃拉帕沙中间体1-α的制备方法
标题:一种沃拉帕沙中间体1-α的制备方法
摘要:本发明提供了一种沃拉帕沙中间体1‑α的制备方法,属于化学药物合成技术领域.包括以下步骤:1)步骤一:高温下,在苯甲醚溶剂中,化合物2发生分子内狄尔斯‑阿尔德环化反应,主要反应生成外型加成产物3‑exo‑a;2)步骤二:步骤一所得固体混合物悬浮于异丙醇,乙醇,甲苯混合溶剂中,加入催化量三乙胺,加热,固体混合物逐渐溶解,梯度降温析晶,经过动态拆分重结晶得到1‑α.本发明方法产率高,质量稳定可控,操作简洁,成本低,适合产业化生产.

专利信息

专利号:US-8618314-B2
优先权日:2005-01-14
标 题 :Exo- and diastereo-selective synthesis of himbacine analogs
发明人：WU GEORGE G; SUDHAKAR ANANTHA; WANG TAO; XIE JI; CHEN FRANK X; POIRIER MARC; HUANG MINGSHENG; SABESAN VIJAY; KWOK DAW-LONG; CUI JIAN; YANG XIAOJING; THIRUVENGADAM TIRUVETTIPURAM K; LIAO JING; ZAVIALOV ILIA; NGUYEN HOA N; LIM NGIAP KIE
权利人:WU GEORGE G; SUDHAKAR ANANTHA; WANG TAO; XIE JI; CHEN FRANK X; POIRIER MARC; HUANG MINGSHENG; SABESAN VIJAY; KWOK DAW-LONG; CUI JIAN; YANG XIAOJING; THIRUVENGADAM TIRUVETTIPURAM K; LIAO JING; ZAVIALOV ILIA; NGUYEN HOA N; LIM NGIAP KIE; MERCK SHARP & DOHME
摘要:This application discloses a novel process for the preparation of himbacine analogs useful as thrombin receptor antagonists. The process is based in part on the use of a base-promoted dynamic epimerization of a chiral nitro center. The chemistry taught herein can be exemplified by the following:

专利号:US-8258319-B2
优先权日:2005-01-14
标 题:Exo- and diastereo- selective synthesis of himbacine analogs

专利号:US-2011251392-A1
优先权日:2005-01-14
标 题:Exo- and diastereo- selective synthesis of himbacine analogs

专利号:US-2012296093-A1
优先权日:2005-01-14
标题 :Exo- and diastereo- selective synthesis of himbacine analogs