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    Process for preparation of pentostatin (R)-3-(2-Deoxy-beta-D-erythro-pentofuranosyl)-3,6,7,8-tetrahydroimidaz[4,5-d][1,3] diazepin-8-ol
    9.
    发明申请
    Process for preparation of pentostatin (R)-3-(2-Deoxy-beta-D-erythro-pentofuranosyl)-3,6,7,8-tetrahydroimidaz[4,5-d][1,3] diazepin-8-ol 审中-公开
    制备喷他他汀（R）-3-（2-脱氧-β-D-赤型 - 呋喃戊糖基）-3,6,7,8-四氢咪唑并[4,5-d] [1,3]二氮杂-8- ol

    公开(公告)号：US20090012288A1

    公开(公告)日：2009-01-08

    申请号：US11822177

    申请日：2007-07-03

    申请人： Hai-Ren Zhang ,  Wuyi Wang

    发明人： Hai-Ren Zhang ,  Wuyi Wang

    IPC分类号： C07D473/00

    CPC分类号： C07D487/04

    摘要： In a process for preparing pentostatin, the improvement wherein reduction is performed on ketone prior to deprotection, comprising: a) reacting 3-(2-deoxy-3,5-di-O-p-toluoyl-b-D-erythro-pentofuranosyl)-6,7-dihydroimidazol [4,5-d][1,3] diazepin-8 (3H)-one with a ruthenium catalyst formed by the reaction of di-μ-chlorobis[(p-cymene) chlororuthenium (II) and N-(arylsulfonyl)-1,2-diarylethylene diamine in a solvent; b) stopping the reaction in step a) by making the reaction medium alkaline; c) separating the mixture from step b) into combined organic layers and washing the reaction product from the combined organic layers with water, filtering, and evaporating solvent to provide a crude product, wherein the ratio of 8R vs 8S isomeric alcohol >100; d) purifying said crude product by chromatography; e) deprotecting the keto nucleoside in the crude product in methanol/sodium methoxide to obtain pentostatin; and f) purifying by recrystallizing pentostatin from methanol to remove inorganic and isomeric impurities.

    摘要翻译： 在制备喷司他丁的方法中，其改进在于在脱保护之前还原在酮上进行，包括：a）使3-（2-脱氧-3,5-二 - 对甲苯酰基-bD-赤型 - 戊呋喃糖基） 通过二氯双[（对甲基异丙基苯）氯钌（II）和N-甲基苯甲酰胺反应形成的钌催化剂，将7-二氢咪唑并[4,5-d] [1,3]二氮杂-8（3H） （芳基磺酰基）-1,2-二亚乙基二胺在溶剂中; b）在步骤a）中停止反应，使反应介质呈碱性; c）将步骤b）中的混合物分离成合并的有机层，并从合并的有机层中用水，过滤和蒸发溶剂洗涤反应产物，得到粗产物，其中8R与8S异构醇的比> 100; d）通过色谱纯化所述粗产物; e）将甲醇/甲醇钠中的粗产物中的酮基核苷脱保护，得到喷司他丁; 和f）通过从甲醇中重结晶pentostatin来除去无机和异构杂质的纯化。