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    • 1. 发明公开
    • Intermediates for the Synthesis of Vitamin D
    • Zwischenproduktefürdie Synthese von维生素D
    • EP1031552A1
    • 2000-08-30
    • EP00102948.7
    • 2000-02-14
    • F. HOFFMANN-LA ROCHE AG
    • Daniewski, Andrzej Robert
    • C07C45/63C07C45/62C07C49/477
    • C07C45/62C07C45/63C07C49/443C07C49/477
    • The invention relates to an improved process for preparing [(3aR,4S,7aS)-4-bromooctahydro-7a-methyl-1H-indene-1,5-dione]. (S)-(+)-2,3,7,7a-tetrahydro-7a-methyl-1H-indene-1,5(6H)-dione is reduced by reaction with diisobutylaluminum hydride and hexamethylphosphoric triaminde in the presence of a catalyst of the formula R-Cu, wherein R is
      and R 1 , R 2 and R 3 are each, independently, selected from the group consisting of C 1 - 7 alkyl, phenyl, phenyl substituted by at least one C 1 - 4 alkyl group, benzyl, or benzyl substituted by at least one C 1 - 4 alkyl groups to form a reductate. The reductate is then treated with a bromine-containing electrophile to yield (3aR,4S,7aS)-4-bromooctahydro-7a-methyl-1H-indene-1,5-dione.
    • 本发明涉及制备Ä(3aR,4S,7aS)-4-溴八氢-7a-甲基-1H-茚-1,5-二酮的改进方法。 (S) - (+) - 2,3,7,7a-四氢-7a-甲基-1H-茚-1H(6H) - 二酮在催化剂存在下与氢化二异丁基铝和六甲基磷酸三 的式R-Cu,其中R是,R 1,R 2和R 3各自独立地选自C 1-7烷基,苯基,被 至少一个C 1-4烷基,苄基或被至少一个C 1-4烷基取代的苄基以形成还原剂。 然后用含溴亲电子试剂处理还原物,得到(3aR,4S,7aS)-4-溴八氢-7a-甲基-1H-茚-1,5-二酮。