HRID1253270

反应详情

EQUATION

反应方程式

HRID 1253270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,2-Dimethylcyclopentane-1,3-dicarboxylic anhydride (1.68 g., 10 mmole) and 1-(4-aminobutyl)-4-(6-chloro-2-pyrazinyl)piperazine (2.97 g., 11 mmole) were combined in 500 ml. of xylene and refluxed for 48 hours with Dean-Stark water removal. Concentration in vacuum, column chromatography on 100 g. of silica gel with chloroform, and recrystallization from 50 ml. of isopropanol with addition of 4N isopropanolic HCl gave 0.55 g. of the title compound as the monohydrochloride; m.p. 210° C. (d).

WORKUP

后处理

  1. concentrationConcentration in vacuum, column chromatography on 100 g
  2. customof silica gel with chloroform, and recrystallization from 50 ml
  3. additionof isopropanol with addition of 4N isopropanolic HCl
  4. customgave 0.55 g