HRID278620

反应详情

EQUATION

反应方程式

HRID 278620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-(trans-4-aminocyclohexane-1-ylcarbonyl)-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (100 mg) and triethylamine (120 mg) in ethanol (10 ml) was added 2-methylthioimidazoline (116 mg), and the mixture was heated for 48 hours under reflux. The reaction solution was concentrated, and the residue was purified with silica gel column chromatography (dichloromethane/methanol containing 10% ammonia=10/1) and transformed into hydrochloride with 4 N hydrochloric acid in ethyl acetate to give a colorless solid of the title compound (30 mg).

WORKUP

后处理

  1. temperaturethe mixture was heated for 48 hours
  2. temperatureunder reflux
  3. concentrationThe reaction solution was concentrated
  4. customthe residue was purified with silica gel column chromatography (dichloromethane/methanol containing 10% ammonia=10/1)