HRID1875439

反应详情

EQUATION

反应方程式

HRID 1875439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2.50 g (12.1 mmol) of ethyl amino(pyridin-2-yl)acetate [G. van Zyl et al., J. Org. Chem. 1961, 26, 3373] are introduced into 20 ml of dichloromethane and, after addition of 4.9 ml (60.3 mmol) of pyridine, cooled to 0° C. A solution of 1.86 g (12.1 mmol) of (2-fluorophenyl)acetyl chloride is then slowly added, and the mixture is stirred at 0° C. for 30 min and then at RT for 2 h. It is diluted with ethyl acetate, washed with sodium bicarbonate solution and dried over sodium sulfate. The crude product is purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 1:1). 2.9 g (76% of theory) of the desired product are obtained.

WORKUP

后处理

  1. waitat RT for 2 h
  2. washwashed with sodium bicarbonate solution
  3. dry with materialdried over sodium sulfate
  4. customThe crude product is purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 1:1)