HRID266156

反应详情

EQUATION

反应方程式

HRID 266156 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 (1.78 g), tert-butylamine (17.4 g) and dichloromethane (40 ml) was stirred at room temperature for 13 hours. The reaction mixture was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with dichloromethane-ethanol (30:1, v/v) gave 2-(tert-butylaminomethyl)-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (0.77 g, 40%). This compound was recrystallized from ethyl acetate - hexane. Colorless prisms, mp. 120°-122° C.

WORKUP

后处理

  1. washThe reaction mixture was washed with water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. washThe fractions eluted with dichloromethane-ethanol (30:1