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