HRID255680

反应详情

EQUATION

反应方程式

HRID 255680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Acetaminobenzene sulfonyl chloride (23.3 g, 0.1 mole) as a slurry in 400 ml methylene chloride was added to N,N'-diisopropyl ethylene diamine (14.46 g, 0.1 mole) and triethylamine (10.1 g, 0.1 mole) in methylene chloride (600 ml). The reaction was stirred overnight at room temperature. The reaction was washed with water, insoluble by-product filtered off, and the filtrate stripped to a brown gum. After filtration through silica gel in 20% MeOH/EtOAc the crude crystalline product was recrystallized from isopropanol to provide the title product as the hydrochloride salt (3.00 g, m.r. 176°-178° C.).

WORKUP

后处理

  1. washThe reaction was washed with water, insoluble by-product
  2. filtrationfiltered off
  3. filtrationAfter filtration through silica gel in 20% MeOH/EtOAc the crude crystalline product
  4. customwas recrystallized from isopropanol