HRID1242256

反应详情

EQUATION

反应方程式

HRID 1242256 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

A mixture of 25 g (0.11 mol) N-(2′-chloro-6′-fluorophenyl)-4-methylaniline and 40 ml (0.5 mol) of chloroacetylchloride is heated under a nitrogen atmosphere for 15 minutes at 60°. The solvent is evaporated under reduced pressure to give an oil which is dissolved in 25 ml of ethyl acetate. Pentane (250 ml) is added dropwise over 15 minutes to precipitate the product. The mixture is cooled to −15° C. and the solid is filtered and washed with pentane to give N-(2′-chloro-6′-fluorophenyl)-N-chloroacetyl-4-methylaniline, m.p. 80–83°.

WORKUP

后处理

  1. temperatureis heated under a nitrogen atmosphere for 15 minutes at 60°
  2. customThe solvent is evaporated under reduced pressure
  3. customto give an oil which
  4. customto precipitate the product
  5. filtrationthe solid is filtered
  6. washwashed with pentane