HRID745211

反应详情

EQUATION

反应方程式

HRID 745211 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of cis-4-cyclohexene-1,2-dicarboxylic anhydride (633 mg; 4.25 mmol), 1-(4-aminobutyl)-4-(2-pyrimidinyl)piperazine (1 g; 4.25 mmol) and n-butanol (10 ml) was heated under reflux for 6 hours. The solvent was removed under reduced pressure, and the residue was purified by silica gel chromatography to give an oily substance. The oily substance was treated with a mixture of 3% hydrogen chloride in isopropanol, and the precipitate was recrystallized from isopropanol to give N-[4-{4-(2-pyrimidinyl)-1-piperazinyl}butyl]-4-cyclohexene-1,2-dicarboximide hydrochloride. M.P., 177°-179° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. customThe solvent was removed under reduced pressure
  4. customthe residue was purified by silica gel chromatography
  5. customto give an oily substance
  6. customthe precipitate was recrystallized from isopropanol