HRID49298

反应详情

EQUATION

反应方程式

HRID 49298 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 1,4-bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (72.4 g, 0.120 mol) in ethanol-chloroform (1:3, 600 mL) was added methanesulfonic acid (24.9 g, 0.258 mol), and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a slightly yellow crystalline powder (melting point: 204.0-206.0° C.) (88.2 g, yield: 92%).

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe residue was recrystallized from methanol-diethyl ether