HRID1605516

反应详情

EQUATION

反应方程式

HRID 1605516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-amino-3-mercapto-4-phenoxybenzoic acid (2.6 g) in saturated sodium hydrogen carbonate (120 ml) is cooled to 4° C. While cooling and stirring, allyl bromide (1 g) is added, and the reaction mixture is kept under nitrogen. After additional stirring for 10 minutes, 3-allylthio-5-amino-4-phenoxybenzoic acid is precipitated by addition of hydrochloric acid until pH 3. After collection by filtration, recrystallisation from aqueous ethanol, and drying in vacuo, the compound is obtained with a melting point of 142°-143° C.

WORKUP

后处理

  1. temperatureWhile cooling
  2. stirringAfter additional stirring for 10 minutes
  3. custom3-allylthio-5-amino-4-phenoxybenzoic acid is precipitated by addition of hydrochloric acid until pH 3
  4. customAfter collection
  5. filtrationby filtration, recrystallisation from aqueous ethanol
  6. customdrying in vacuo
  7. customthe compound is obtained with a melting point of 142°-143° C.