HRID2245429
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
To a solution of the methyl (3S)-3-hydroxy-L-prolinate hydrochloride (D68, 1.8 g, 9.9 mmol) and Et3N (3 ml, 21.8 mmol) in 10 ml of dry benzene at the temperature of 7-8 ° C. was added dropwise a solution of chloroacetyl chloride (0.87 ml, 10.9 mmol) in 5 ml of dry benzene. After 24 h at rt, the precipitated was filtered off and washed with AcOEt. The filtrate was evaporated, and the crude oil was purified by flash chromatography column (Cy/AcOEt ¼ as eluent). The title compound was isolated as a colourless oil (1.48 g). Yield 67%.
WORKUP
后处理
- filtrationthe precipitated was filtered off
- washwashed with AcOEt
- customThe filtrate was evaporated
- customthe crude oil was purified by flash chromatography column (Cy/AcOEt ¼ as eluent)