HRID1606600

反应详情

EQUATION

反应方程式

HRID 1606600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,4-dichloro-5-methylsulfonylbenzoic acid (6.0 g.; 0.0224 mole), butylamine (9 ml.) and ethyl cellosolve (20 ml.) is heated at reflux in a nitrogen atmosphere for 5 hours. The solvent is distilled at reduced pressure and the residue is dissolved in water (75 ml.) then treated with dilute hydrochloric acid which causes the product to precipitate. After recrystallization from butyl chloride there is collected 2.3 g. (34% yield) of 2-butylamino-4-chloro-5-methylsulfonylbenzoic acid, m.p. 187°-9° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux in a nitrogen atmosphere for 5 hours
  3. distillationThe solvent is distilled at reduced pressure
  4. dissolutionthe residue is dissolved in water (75 ml.)
  5. additionthen treated with dilute hydrochloric acid which
  6. customto precipitate
  7. customAfter recrystallization from butyl chloride
  8. customthere is collected 2.3 g