HRID839862
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 10 g of 2-benzoyl-cyclohexanone, 5.8 g of pyruvic acid and 0.2 g of sodium dodecylsulfate is heated at 150° for 15 hours. After cooling, the raw reaction product is extracted with ethyl ether and the ether solution is washed with an aqueous solution of sodium bicarbonate, then with water and then dried. The residue which is obtained after removing the solvent (9 g) is chromatographed on an SiO2 column using as an eluent cyclohexane: ethyl ether 7:3. There are obtained 3.2 g of 7-benzoyl-3-methyl-2,4,5,6-tetrahydro-benzo[b]furan-2-one. After recrystallization from hexane-ethyl acetate m.p. is 79°-81°.
WORKUP
后处理
- temperatureis heated at 150° for 15 hours
- temperatureAfter cooling
- customthe raw reaction product
- extractionis extracted with ethyl ether
- washthe ether solution is washed with an aqueous solution of sodium bicarbonate
- dry with materialwith water and then dried
- customThe residue which is obtained
- customafter removing the solvent (9 g)
- customis chromatographed on an SiO2 column