HRID436929

反应详情

EQUATION

反应方程式

HRID 436929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

p-(Cyclobutylcarbonyl)phenylacetonitrile (8.1 g) in ethanol (50 ml) was added to potassium hydroxide (6.8 g) in water (50 ml) and the mixture was heated under reflux for 5 hours and cooled. The solution was diluted with water (100 ml), washed with ether (2× 100 ml), acidified to pH 1 with hydrochloric acid and extracted with ether (3× 100 ml). The combined extracts were dried over magnesium sulphate, filtered and evaporated to give a brown oil. This was extracted with a hot mixture of light petroleum (b.p. 60°-80°) and ethyl acetate (9:1) (3× 200 ml). The solid that crystallised from the extracts on cooling was collected. It had m.p. 91°-92.5°.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. temperaturecooled
  4. washwashed with ether (2× 100 ml)
  5. extractionextracted with ether (3× 100 ml)
  6. dry with materialThe combined extracts were dried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated
  9. customto give a brown oil
  10. extractionThis was extracted with a hot mixture of light petroleum (b.p. 60°-80°) and ethyl acetate (9:1) (3× 200 ml)
  11. customThe solid that crystallised from the extracts
  12. temperatureon cooling
  13. customwas collected