HRID1577357

反应详情

EQUATION

反应方程式

HRID 1577357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 261.8 g of 3-methoxybromobenzene in 500 ml of ether is added dropwise to a 34.0 g sample of magnesium in 600 ml of ether. To the reaction mixture is added a suitable catalyst and the mixture is heated vigorously to initiate the reaction. The prepared Grignard Reagent is cooled in an ice bath while 185.6 g of 2-chlorocyclohexanone in 500 ml of ether is introduced. The ether is removed and xylene added and the xylene solution is refluxed for 1 hour. The solution is poured over ice and dilute hydrochloric acid, the organic layer separated, the aqueous layer extracted with benzene, the organic layer and benzene extracts are combined and washed with dilute sodium hydroxide solution, dried, filtered, and the solvent removed leaving a red oil. The oil is vacuum distilled to give a clear pink liquid of 2-(3-methoxyphenyl)cyclohexanone.

WORKUP

后处理

  1. additionTo the reaction mixture is added a suitable catalyst
  2. temperaturethe mixture is heated vigorously
  3. customthe reaction
  4. additionis introduced
  5. customThe ether is removed
  6. additionxylene added
  7. temperaturethe xylene solution is refluxed for 1 hour
  8. additionThe solution is poured over ice and dilute hydrochloric acid
  9. customthe organic layer separated
  10. extractionthe aqueous layer extracted with benzene
  11. washwashed with dilute sodium hydroxide solution
  12. customdried
  13. filtrationfiltered
  14. customthe solvent removed
  15. customleaving a red oil
  16. distillationdistilled