HRID267793

反应详情

EQUATION

反应方程式

HRID 267793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-chlorosalicylaldehyde (78 g., 0.5 mole), finely powdered anhydrous potassium carbonate (103.5 g., 0.75 mole) and acetone (500 ml.) is stirred under reflux and 2-chloropropionitrile (33.6 g., 0.375 mole) is added over a period of about 5 minutes. The mixture is heated under reflux for 1.5 hours and then treated with potassium carbonate (34.5 g., 0.25 mole) followed by more 2-chloropropionitrile (11.2 g., 0.125 mole). Heating and stirring are continued for 31/2 hours, after which the reaction mixture is filtered and the filter-cake washed with acetone. Evaporation of the combined filtrate gives 3-chloro-6-(1-cyanoethoxy)-benzaldehyde which is recrystallized from aqueous methanol.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 1.5 hours
  4. temperatureHeating
  5. stirringstirring
  6. custom2 hours
  7. filtrationafter which the reaction mixture is filtered
  8. washthe filter-cake washed with acetone
  9. customEvaporation of the combined filtrate