HRID724782

反应详情

EQUATION

反应方程式

HRID 724782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 1-(3-trifluoromethoxyphenyl)-3-hydroxy-2-pyrrolidone (19.42 g) in dichloromethane (250 ml) was cooled in an ice bath and treated with triethylamine (11.32 ml). Methanesulfonyl chloride (6.05 ml) was added dropwise via a syringe, and the mixture stirred with cooling for a further 1 hour after which it was allowed to warm to room temperature. After stirring for 2 hours at room temperature methanesulfonyl chloride (0.5 ml) and triethylamine (1.0 ml) were added and the mixture was stirred for a further 2 hours. The reaction mixture was poured into water and extracted with dichloromethane. The dichloromethane extracts were washed with water, dried (MgSO4) and the solvent evaporated under reduced pressure to give the crude sub-title compound (23.0 g), which was used without further purification.

WORKUP

后处理

  1. temperaturewith cooling for a further 1 hour after which it
  2. additionwere added
  3. stirringthe mixture was stirred for a further 2 hours
  4. extractionextracted with dichloromethane
  5. washThe dichloromethane extracts were washed with water
  6. dry with materialdried (MgSO4)
  7. customthe solvent evaporated under reduced pressure