HRID1910760

反应详情

EQUATION

反应方程式

HRID 1910760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Thionyl chloride (3 mL, 41 mmol) was added to 2-methyl-2-(4-nitrophenyl)-propionic acid (1 g, 4.78 mmol) and heated at 90° C. overnight. Excess thionyl chloride was evaporated to give a crude acid chloride which was dissolved in acetonitrile (8 mL). To this was added 2-bromoethanol (0.41 mL, 5.78 mmol) then the mixture was heated at reflux overnight. After concentration in vacuo, the residue was diluted with ethyl acetate and washed with sodium bicarbonate solution, then the organic layer was dried and evaporated to afford 2-methyl-2-(4-nitrophenyl)-propionic acid, 2-bromo-ethyl ester (0.99 g, 65.5%).

WORKUP

后处理

  1. customExcess thionyl chloride was evaporated
  2. customto give a crude acid chloride which
  3. temperaturethe mixture was heated
  4. temperatureat reflux overnight
  5. concentrationAfter concentration in vacuo
  6. additionthe residue was diluted with ethyl acetate
  7. washwashed with sodium bicarbonate solution
  8. customthe organic layer was dried
  9. customevaporated