HRID1576208
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
A mixture of 17.54 g. (0.058 mole) of 4-cyano-4-(3,4-dimethoxy)cyclohexanone, ethylene ketal (prepared as in Example 22) and 17.5 g. of potassium hydroxide in 175 ml. of ethylene glycol is heated at reflux for about 16 hours. The resulting solution is allowed to cool, diluted with water and washed with ether. The aqueous layer is covered with ether and then cautiously acidified. The aqueous layer is extracted with two additional portions of ether and the extracts combined. The extracts are evaporated to dryness to give 19 g. (99% yield) of 4-carboxy-4-(3,4-dimethoxyphenyl)cyclohexanone, ethylene ketal, as an amorphous gum.
WORKUP
后处理
- additionA mixture of 17.54 g
- temperatureat reflux for about 16 hours
- temperatureto cool
- washwashed with ether
- extractionThe aqueous layer is extracted with two additional portions of ether
- customThe extracts are evaporated to dryness
- customto give 19 g