HRID1105744

反应详情

EQUATION

反应方程式

HRID 1105744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-[N-methyl-N-(7-chloro-1,2,4-benzotriazin-3-yl)amino]phenol (1.5 g; Example 6 part (a)), ethyl 2-bromo-2-methylpropionate (1.23 g), anhydrous potassium carbonate (0.87 g) and dimethylformamide (15 ml) was heated, with stirring, at a temperature of 100° C. for a period of 3 days. The cooled solution was poured into dichloromethane and the mixture was washed with water. The aqueous phase was dried (over anhydrous magnesium sulfate) and the solvent was removed by distillation under reduced pressure to give an oil. The crude product was purified by chromatography over silica gel (eluent dichloromethane) to give the title compound (0.9 g) as a red oil.

WORKUP

后处理

  1. temperaturewas heated
  2. washthe mixture was washed with water
  3. dry with materialThe aqueous phase was dried (over anhydrous magnesium sulfate)
  4. customthe solvent was removed by distillation under reduced pressure
  5. customto give an oil
  6. customThe crude product was purified by chromatography over silica gel (eluent dichloromethane)