HRID1287692

反应详情

EQUATION

反应方程式

HRID 1287692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A 19.9 g (0.1 mol) portion of o-methylbenzoyl bromide was added dropwise with cooling to a mixture of 13.7 g (0.1 mol) of o-ethoxyaniline and 8.4 g (0.1 mol) of sodium bicarbonate in 200 ml of acetone with stirring. After addition of the o-methylbenzoyl bromide, the reaction mixture was warmed to 40° C and the mixture was refluxed and stirred for another 40 hours. After filtering, the ether was distilled from the reaction mixture and the residual material was re-dissolved in ether and washed with water. The ether layer was dried over anhydrous sodium sulfate, the ether was removed and the product was distilled to obtain 24.1 g (94.5%) of a clear pink liquid having a boiling point of 148° C/0.04 mm Hg and nD20 of 1.5929.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. stirringstirred for another 40 hours
  3. filtrationAfter filtering
  4. distillationthe ether was distilled from the reaction mixture
  5. dissolutionthe residual material was re-dissolved in ether
  6. washwashed with water
  7. dry with materialThe ether layer was dried over anhydrous sodium sulfate
  8. customthe ether was removed
  9. distillationthe product was distilled