HRID1282786

反应详情

EQUATION

反应方程式

HRID 1282786 的结构方程式

PROCEDURE

实验过程

3-Benzylthio-5-chlorosulfonyl-4-phenoxybenzoic acid (0.6 g) is added to concentrated aqueous ammonia (10 ml). After 1 hour, the reaction mixture is heated on a steam-bath for 15 minutes, and crude 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid until pH 2.5. The crude product is dissolved in aqueous sodium hydrogen carbonate by heating. After cooling, the precipitated sodium salt of 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration. The salt is redissolved in hot water (20 ml) and 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid. After cooling and collecting by filtration, and drying in vacuo at 80°C, the compound is obtained with a melting point of 235°-236°C.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated on a steam-bath for 15 minutes
  2. customcrude 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid until pH 2.5
  3. dissolutionThe crude product is dissolved in aqueous sodium hydrogen carbonate
  4. temperatureby heating
  5. temperatureAfter cooling
  6. filtrationthe precipitated sodium salt of 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration
  7. dissolutionThe salt is redissolved in hot water (20 ml)
  8. custom3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid
  9. temperatureAfter cooling
  10. filtrationcollecting by filtration
  11. customdrying in vacuo at 80°C
  12. customthe compound is obtained with a melting point of 235°-236°C.