HRID1648456

反应详情

EQUATION

反应方程式

HRID 1648456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 158 g of 3-chlorobenzaldehyde, 111.6 g of trimethylsilylnitrile and a catalytic amount of zinc iodide was heated at 90° C. for 2 hours, with stirring. The reaction mixture was ice-cooled, and 350 ml of concentrated aqueous hydrochloric acid were added to it. The resulting mixture was then heated under reflux for one hour, after which it was mixed with water and with ethyl acetate. The ethyl acetate layer was separated and mixed with a 30% w/v aqueous solution of sodium hydroxide. The aqueous layer was separated, washed three times with ethyl acetate and then acidified with concentrated aqueous hydrochloric acid, after which it was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by distillation under reduced pressure, to give 172 g of the title compound as crystals, melting at between 110° C. and 114° C.

WORKUP

后处理

  1. temperaturecooled
  2. temperatureThe resulting mixture was then heated
  3. temperatureunder reflux for one hour
  4. customThe ethyl acetate layer was separated
  5. additionmixed with a 30% w/v aqueous solution of sodium hydroxide
  6. customThe aqueous layer was separated
  7. washwashed three times with ethyl acetate
  8. extractionafter which it was extracted with ethyl acetate
  9. washThe extract was washed with water
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was then removed by distillation under reduced pressure