HRID355121

反应详情

EQUATION

反应方程式

HRID 355121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-5-chlorosulfonyl benzoic acid, 3.5 g. (0.014 mole), is added to a solution of 2-(p-chlorophenyl)ethylamine, 6.5 g. (0.042 mole) in 25 ml. methylene chloride. The resulting slurry is stirred overnight and filtered to recover 9.7 g. of residue. This is recrystallized three times from aqueous isopropanol, then dissolved in 1 N aqueous sodium hydroxide, washed three times with ether, and then acidified with conc. hydrochloric acid. The resulting precipitate is recrystallized twice from aqueous isopropanol to yield the desired product, m.p. 176°-178° C.

WORKUP

后处理

  1. filtrationfiltered
  2. customto recover 9.7 g
  3. customThis is recrystallized three times from aqueous isopropanol
  4. dissolutiondissolved in 1 N aqueous sodium hydroxide
  5. washwashed three times with ether
  6. customThe resulting precipitate is recrystallized twice from aqueous isopropanol