HRID266154

反应详情

EQUATION

反应方程式

HRID 266154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (10.0 g), ethylamine (70% aqueous solution, 206 g) and ethanol (200 ml)--dichloromethane (200 ml) was stirred at room temperature for 13 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in dichloromethane. The dichloromethane layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform - ethanol (5:1, v/v) gave 2-(N-ethylaminomethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (5.7 g, 55%). This compound was recrystallized from ethanol. Colorless prisms, mp. 128°-130° C.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in dichloromethane
  3. washThe dichloromethane layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. washThe fractions eluted with chloroform - ethanol (5:1