HRID2245429

反应详情

EQUATION

反应方程式

HRID 2245429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationthe precipitated was filtered off
  2. washwashed with AcOEt
  3. customThe filtrate was evaporated
  4. customthe crude oil was purified by flash chromatography column (Cy/AcOEt ¼ as eluent)