HRID323280
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
- -5 °C
PROCEDURE
实验过程
Combine 1-(3,4,5-trimethoxybenzyl)-3-(4-fluorophenylmethyl)-3-(3-hydroxypropyl)-2-oxopyrrolidine (2.6 mmol), and dichloromethane (15 mL). Cool to −5° C. using a salt-ice bath. Add dropwise, methanesulfonyl chloride (0.19 g, 1.62 mmol) at such a rate as to maintain the reaction temperature below 0° C. After 1 hour, the reaction mixture is extracted with 1 M hydrochloric acid solution and then a 5% sodium bicarbonate solution. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give the title compound: Rf=0.71 (silica gel, ethyl acetate).
WORKUP
后处理
- additionAdd dropwise
- extractionthe reaction mixture is extracted with 1 M hydrochloric acid solution
- dry with materialDry the organic layer over Na2SO4
- filtrationfilter
- customevaporate in vacuo