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
N-benzenesulfonylglycyl-L-proline benzylester (1.91 g, 4.7 mmole) was dissolved in methanol (6 ml), 1N aqueous sodium hydrochloride (6 ml) was added, and stirred for 3 hours at a temperature between 30° C. and 35° C. Water (20 ml) was added to the solution and the mixture was washed with two 20 ml portions of diethyl ether and then adjusted to pH 1.5 with 1N aqueous hydrochloric acid. The solvent was removed by distillation under reduced pressure and the solid material thus obtained was dispersed in ethyl acetate (50 ml) and the mixture was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give a glassy residue and it was recrystallized from ethyl acetate and petroleum ether to obtain N-benzenesulfonylglycyl-L-proline(yield: 0.67 g, 45.2%).
WORKUP
后处理
- washthe mixture was washed with two 20 ml portions of diethyl ether
- customThe solvent was removed by distillation under reduced pressure
- customthe solid material thus obtained
- dry with materialthe mixture was dried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customto give a glassy residue and it
- customwas recrystallized from ethyl acetate and petroleum ether