HRID1780666

反应详情

EQUATION

反应方程式

HRID 1780666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1.54 g portion of 2-chlorobenzoxazole was dissolved in 5 ml of dichloromethane. Under cooling with ice, to this was added dropwise 2.28 g of N-methylhomopiperazine which had been dissolved in 10 ml of dichloromethane, followed by 1 hour of reaction. The reaction solution was concentrated under a reduced pressure, and the resulting residue was dissolved in 500 ml of dichloromethane, washed with water, dehydrated with sodium sulfate and then concentrated under a reduced pressure. Thereafter, the resulting residue was purified by a silica gel column chromatography (chloroform:methanol=10:1) to obtain 1.87 g of the title compound.

WORKUP

后处理

  1. temperatureUnder cooling with ice
  2. customfollowed by 1 hour of reaction
  3. concentrationThe reaction solution was concentrated under a reduced pressure
  4. dissolutionthe resulting residue was dissolved in 500 ml of dichloromethane
  5. washwashed with water
  6. concentrationconcentrated under a reduced pressure
  7. customThereafter, the resulting residue was purified by a silica gel column chromatography (chloroform:methanol=10:1)