HRID1287737

反应详情

EQUATION

反应方程式

HRID 1287737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-chloro-3-nitro-5-sulphamyl-benzoic acid (22.4 g), β-phenylethylamine (29 g), and water (200 ml) was refluxed for 2.5 hours. After cooling, the reaction mixture was adjusted to a pH of 9.5 and extracted with diethyl ether. The aqueous layer was then acidified by addition of 4N hydrochloric acid, and the precipitated 3-nitro-4-(β-phenylethylamino)-5-sulphamyl-benzoic acid was collected by suction. After recrystallization from aqueous ethanol, the melting point was 208°-208.5° C.

WORKUP

后处理

  1. temperaturewas refluxed for 2.5 hours
  2. temperatureAfter cooling
  3. extractionextracted with diethyl ether
  4. additionThe aqueous layer was then acidified by addition of 4N hydrochloric acid
  5. customthe precipitated 3-nitro-4-(β-phenylethylamino)-5-sulphamyl-benzoic acid was collected by suction
  6. customAfter recrystallization from aqueous ethanol