HRID1385774

反应详情

EQUATION

反应方程式

HRID 1385774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 390 mg (1.6 mmol) D-Proline benzyl ester hydrochloride and 0.47 ml (3.4 mmol) triethylamine in 20 ml dichloromethane at 0° C. was added dropwise 0.2 ml (2.4 mmol) acryloyl chloride and stirring continued for 24 h at room temperature. The reaction mixture was then washed sequentially with water, 1 M hydrochloric acid and once more with water, and the aqueous phases back-extracted with dichloromethane. The combined organic extracts were dried over sodium sulfate and concentrated in vacuo to afford 420 mg (100%) of the title compound as a colorless oil. MS m/e (%): 259 (M+, 25), 124 (100), 91 (25), 70 (21).

WORKUP

后处理

  1. washThe reaction mixture was then washed sequentially with water, 1 M hydrochloric acid and once more with water
  2. extractionthe aqueous phases back-extracted with dichloromethane
  3. dry with materialThe combined organic extracts were dried over sodium sulfate
  4. concentrationconcentrated in vacuo