HRID436929
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureunder reflux for 5 hours
- temperaturecooled
- washwashed with ether (2× 100 ml)
- extractionextracted with ether (3× 100 ml)
- dry with materialThe combined extracts were dried over magnesium sulphate
- filtrationfiltered
- customevaporated
- customto give a brown oil
- extractionThis was extracted with a hot mixture of light petroleum (b.p. 60°-80°) and ethyl acetate (9:1) (3× 200 ml)
- customThe solid that crystallised from the extracts
- temperatureon cooling
- customwas collected