首页> 外国专利> A PROCESS FOR THE ISOLATION OF CRYSTALS OF OPTIONALLY SUBSTITUTED 2-(2-PYRIDINYL)METHYLTHIO-1H-BENZIMIDAZOLE HYDRATES

A PROCESS FOR THE ISOLATION OF CRYSTALS OF OPTIONALLY SUBSTITUTED 2-(2-PYRIDINYL)METHYLTHIO-1H-BENZIMIDAZOLE HYDRATES

机译:选择性取代的2-(2-吡啶基)甲基硫代-1H-苯并咪唑水合物的晶体分离过程

摘要

"A PROCESS FOR THE ISOLATION OF CRYSTALS OF OPTIONALLY SUBSTITUTED 2-(2-PYRIDINYL)METHYLTHIO-1H-BENZIMIDAZOLE HYDRATES" A process for the isolation of crystals of optionally substituted 2-(2-pyridinyl)methylthio-lH-benzimidazole hydrates of the following structural formula I in which R1, R2 and R3, identical or different, denote hydrogen, a C1—C8 alkyl, C3-C8 cycloalkyl, C2-C8 fluoroalkyl or C1-C8 alkoxy, R4 and R5, identical or different, denote hydrogen, a C1-C8 alkyl, C3-C8 cycloalkyl, CH2- C3—C8 cycloalkyl, C1-C8 alkoxycarbonyl, C1-C8 alkoxy, C1-C8 fluoroalkoxy, CF3-, C2-C8 fluoroalkyl or C(O)O-C1-C8 alkyl and R6 denotes hydrogen or a C1-C2 alkyl and x means 0.5-2; wherein said process comprises isolation from a reaction medium as herein described containing the free base, characterized in that a water-soluble, organic solvent present in the reaction medium is at most partially removed, water is added to the reaction medium at a temperature of below 40°C water in quantities of at least 55 wt.%, relative to the reaction medium, and the hydrates formed are separated as crystals and optionally purified in conventional manner.
机译:“分离被任选取代的2-(2-吡啶基)甲基噻吩-1H-苯并咪唑水合物的晶体的方法”分离该化合物的任选取代的2-(2-吡啶基)甲硫基-1H-苯并咪唑水合物的晶体的方法遵循结构式I,其中R 1,R 2和R 3相同或不同,表示氢,C 1 -C 8烷基,C 3 -C 8环烷基,C 2 -C 8氟代烷基或C 1 -C 8烷氧基,R 4和R 5相同或不同,表示氢,C1-C8烷基,C3-C8环烷基,CH2-C3-C8环烷基,C1-C8烷氧羰基,C1-C8烷氧基,C1-C8氟烷氧基,CF3-,C2-C8氟烷基或C(O)O-C1- C 8烷基,R 6表示氢或C 1 -C 2烷基,x表示0.5-2。其中所述方法包括从如本文所述的包含游离碱的反应介质中分离,其特征在于反应介质中存在的水溶性有机溶剂最多被部分除去,在低于200℃的温度下向反应介质中添加水。相对于反应介质,数量为至少55重量%的40℃水和形成的水合物以晶体形式分离并且任选地以常规方式纯化。

著录项

  • 公开/公告号IN224551B

    专利类型

  • 公开/公告日2009-01-09

    原文格式PDF

  • 申请/专利权人

    申请/专利号IN103/MUMNP/2004

  • 发明设计人

    申请日2004-02-11

  • 分类号C07D401/12;

  • 国家 IN

  • 入库时间 2022-08-21 19:26:48

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