HRID2232580

反应详情

EQUATION

反应方程式

HRID 2232580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

1-(2,3-Dihydro-1,4-benzodioxin-2-ylmethyl)piperazine (2.35 g, 10 mmole), 2,3-dichloropyrazine (1.5 g, 10 mmole) and diisopropylethylamine (1.3 g, 10 mmole) were combined in 100 ml of dimethylformamide and heated at 75° C. under N2 for 24 hours. The solvent was removed in vacuum and the residue was filtered through 75 g of silica gel using choroform as the eluent. The relevant fractions were combined, the solvent evaporated and the residue crystallized from isopropanol with addition of 4N isopropanolic HCl to give 2.1 g of title compound as the hydrochloride, m.p. 217°-218° C.

WORKUP

后处理

  1. customThe solvent was removed in vacuum
  2. filtrationthe residue was filtered through 75 g of silica gel
  3. customthe solvent evaporated
  4. customthe residue crystallized from isopropanol with addition of 4N isopropanolic HCl