HRID1282791

反应详情

EQUATION

反应方程式

HRID 1282791 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Mercapto-4-phenoxy-5-sulfamylbenzoic acid (0.6 g) is suspended in water (20 ml) and the pH is adjusted to 8 by addition of 1 N sodium hydroxide. Benzyl bromide (0.35 g) is added to the resulting solution, and the reaction mixture is stirred for 2 hours at room temperature. After cooling, the precipitated sodium salt of 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration. The salt is dissolved in hot water (60 ml) and the solution acidified by addition of 1 N hydrochloric acid. After cooling, the precipitated 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration and recrystallized from aqueous ethanol to yield the desired compound with a melting point of 234°-236°C., after drying in vacuo.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe precipitated sodium salt of 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration
  3. dissolutionThe salt is dissolved in hot water (60 ml)
  4. additionthe solution acidified by addition of 1 N hydrochloric acid
  5. temperatureAfter cooling
  6. filtrationthe precipitated 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration
  7. customrecrystallized from aqueous ethanol