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
Succinic anhydride (3 g) was added, under a nitrogen atmosphere, to a stirred slurry of aluminium chloride (8.25 g) in 1,2-dichloroethane (50 ml). The resulting mixture was stirred at room temperature for 15 minutes. A solution of 2-acetoxypropyl benzene (5 g) in 1,2-dichloroethane (20 ml) was added, dropwise, to the stirred mixture which was stirred for a further 3 days at room temperature. The reaction mixture was poured into water. The organic solvent was evaporated and the aqueous residue was extracted into ethyl acetate. The organic extract was washed with 2N HCl and extracted into dilute sodium bicarbonate solution. The aqueous extract was acidified with 2N HCl and extracted into ethyl acetate. The organic layer was washed with brine, dried (MgSO4) and evaporated to an oil which was chromatographed on silica gel. Elution with petroleum ether(60-80) - diethyl ether(50:50) gave 3-[4-(2-acetoxypropyl)- benzoyl]propionic acid as an oil.
WORKUP
后处理
- stirringdropwise, to the stirred mixture which was stirred for a further 3 days at room temperature
- customThe organic solvent was evaporated
- extractionthe aqueous residue was extracted into ethyl acetate
- extractionThe organic extract
- washwas washed with 2N HCl
- extractionextracted into dilute sodium bicarbonate solution
- extractionThe aqueous extract
- extractionextracted into ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried (MgSO4)
- customevaporated to an oil which
- customwas chromatographed on silica gel
- washElution with petroleum ether(60-80) - diethyl ether(50:50)