HRID918600

反应详情

EQUATION

反应方程式

HRID 918600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 3-nitro-4-phenoxy-5-sulphamyl-benzoic acid (20 g) in water (100 ml) was adjusted to a pH of 8 by the addition of 1N lithium hydroxide. The resulting solution was hydrogenated at room temperature and 1.1 atmosphere hydrogen pressure, using a palladium-on-carbon catalyst (0.6 g catalyst containing 10% pd). After the hydrogen uptake had become negligible, the catalyst was removed by filtration, and the 3-amino- 4-phenoxy-5-sulphamyl-benzoic acid was precipitated from the filtrate by the addition of 4N hydrochloric acid until the pH was 2.5. After recrystallization from aqueous ethanol and drying, the melting point was 255°-256°C.

WORKUP

后处理

  1. customwas hydrogenated at room temperature
  2. customthe catalyst was removed by filtration
  3. customthe 3-amino- 4-phenoxy-5-sulphamyl-benzoic acid was precipitated from the filtrate by the addition of 4N hydrochloric acid until the pH was 2.5
  4. customAfter recrystallization from aqueous ethanol
  5. customdrying