HRID975712
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
A mixture of (2R,4R)-1-allyloxycarbonyl-4-(t-butyldimethylsilyloxy)-2-(2-methanesulfonyloxyethyl)pyrrolidine (10.0 g) and 1,2,4-triazole sodium salt (2.45 g) in dimethylformamide (50 ml) was stirred at 60° C. for 3.5 hours. After cooling to room temperature, the mixture was quenched by the addition of water (100 ml) and extracted with a mixture of hexane and ethyl acetate (2:1, 50 ml×4). The combined extract was washed with water (400 ml), brine (100 ml) and dried over magnesium sulfate. Evaporation of the solvent gave (2R,4R)-1-allyloxy-carbonyl-4-(t-butyldimethylsilyloxy)-2-[2-(1,2, 4-triazol-1-yl)ethyl]pyrrolidine (8.82 g) as a light brown paste.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customthe mixture was quenched by the addition of water (100 ml)
- extractionextracted with a mixture of hexane and ethyl acetate (2:1, 50 ml×4)
- extractionThe combined extract
- washwas washed with water (400 ml), brine (100 ml)
- dry with materialdried over magnesium sulfate
- customEvaporation of the solvent