HRID2302086

反应详情

EQUATION

反应方程式

HRID 2302086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A mixture of 50.0 g (0.143 mol) of (R)-N-[1-[(3-chlorothien-2-yl )methyl]propyl]-4-methylbenzenesulfonamide lithium salt, prepared as described in PCT/US97/15729, in 50 g methanol is heated with stirring at 65° C. until dissolution of the solids is completed. The solution is cooled to 60° C. and 85 g water is added to the mixture dropwise. The mixture is stirred for 1.5 hours and then cooled to 20° C. The solids are isolated by filtration. Drying under vacuum with nitrogen bleed affords 46.6 g (95%) of the free base (R)-N-[1-[(3-chlorothien-2-yl)methyl]propyl]-4-methylbenzenesulfonamide.

WORKUP

后处理

  1. customprepared
  2. temperatureis heated
  3. temperatureThe solution is cooled to 60° C.
  4. stirringThe mixture is stirred for 1.5 hours
  5. temperaturecooled to 20° C
  6. customThe solids are isolated by filtration
  7. customDrying under vacuum with nitrogen