HRID1658586

反应详情

EQUATION

反应方程式

HRID 1658586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 1.4 g of silver oxide in 20 ml of 6% aqueous sodium hydroxide was added dropwise 2.1 g of the 2-(4-isobutylphenyl)-propionaldehyde obtained in the procedure of Example 3(i) over 10 minutes at 60°C with stirring. The mixture was further stirred at 60°C for 15 minutes and then allowed to stand. The precipitate was filtered off and washed with hot water. The filtrate and the washing liquor were combined together, and the insoluble oil was removed by extracting with ethyl ether. The remaining aqueous phase was then extracted with ethyl ether, and the ether extract was washed with water, dried and then distilled under reduced pressure to remove the ether. The crude crystalline product so obtained was recrystallised from petroleum benzine, affording 1.3 g of 2-(4-isobutylphenyl)-propionic acid, M.P. 74.8°-76.5°C. Yield 57% (based on the theoretical).

WORKUP

后处理

  1. customobtained in the procedure of Example 3(i) over 10 minutes at 60°C
  2. stirringThe mixture was further stirred at 60°C for 15 minutes
  3. filtrationThe precipitate was filtered off
  4. washwashed with hot water
  5. customthe insoluble oil was removed
  6. extractionby extracting with ethyl ether
  7. extractionThe remaining aqueous phase was then extracted with ethyl ether
  8. extractionthe ether extract
  9. washwas washed with water
  10. customdried
  11. distillationdistilled under reduced pressure
  12. customto remove the ether
  13. customThe crude crystalline product so obtained
  14. customwas recrystallised from petroleum benzine