HRID978692

反应详情

EQUATION

反应方程式

HRID 978692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 113.23 g (0.686 mol) of chloral hydrate in 2 liters of water was added 419 g (2.95 mol) of sodium sulfate, followed by a solution prepared from 89.25 g (0.70 mol) of 3-chloroaniline, 62 ml of concentrated hydrochloric acid and 500 ml of water. A thick precipitate formed. To the reaction mixture was then added, with stirring, a solution of 155 g (2.23 mol) of hydroxylamine in 500 ml of water. Stirring was continued and the reaction mixture was warmed slowly and it was maintained between 60 and 75° C. for approximately 6 hours, during which time an additional 1 liter of water had been added to facilitate stirring. The reaction mixture was then cooled and the precipitate was recovered by filtration. The wet solid was dried to give 136.1 g of isonitroso-3-chloroacetanilide.

WORKUP

后处理

  1. customA thick precipitate formed
  2. additionTo the reaction mixture was then added
  3. stirringStirring
  4. temperaturethe reaction mixture was warmed slowly
  5. additionhad been added
  6. stirringto facilitate stirring
  7. temperatureThe reaction mixture was then cooled
  8. filtrationthe precipitate was recovered by filtration
  9. customThe wet solid was dried