HRID2302086
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customprepared
- temperatureis heated
- temperatureThe solution is cooled to 60° C.
- stirringThe mixture is stirred for 1.5 hours
- temperaturecooled to 20° C
- customThe solids are isolated by filtration
- customDrying under vacuum with nitrogen