HRID21680

反应详情

EQUATION

反应方程式

HRID 21680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Briefly, 200 parts of 2,5-dichloro-nitrobenzene were heated to 160° C. and stirred, and 160 parts of the potassium salt of salicylaldehyde was added over a period of 30 minutes. After the addition was complete, an exothermic reaction took place, and the temperature rose to about 195° C. Heating was discontinued until the reaction subsided, and the mixture was heated for 1 hour at 150° C. The mixture was cooled, ice and water were added, and it was extracted with ether. The ether layer was filtered to remove insoluble material, and the resultant solution was dried over sodium sulfate. The ether solvent was evaporated, and the residual oil was re crystallized from a mixture of hexane and benzene to give 2-(2-nitro-4-chloro-phenoxy)benzaldehyde melting at about 100°-101° C.

WORKUP

后处理

  1. additionAfter the addition
  2. customan exothermic reaction
  3. customrose to about 195° C
  4. temperatureHeating
  5. temperatureThe mixture was cooled
  6. extractionit was extracted with ether
  7. filtrationThe ether layer was filtered
  8. customto remove insoluble material
  9. dry with materialthe resultant solution was dried over sodium sulfate
  10. customThe ether solvent was evaporated
  11. customthe residual oil was re crystallized from a mixture of hexane and benzene