HRID465452

反应详情

EQUATION

反应方程式

HRID 465452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringdropwise, to the stirred mixture which was stirred for a further 3 days at room temperature
  2. customThe organic solvent was evaporated
  3. extractionthe aqueous residue was extracted into ethyl acetate
  4. extractionThe organic extract
  5. washwas washed with 2N HCl
  6. extractionextracted into dilute sodium bicarbonate solution
  7. extractionThe aqueous extract
  8. extractionextracted into ethyl acetate
  9. washThe organic layer was washed with brine
  10. dry with materialdried (MgSO4)
  11. customevaporated to an oil which
  12. customwas chromatographed on silica gel
  13. washElution with petroleum ether(60-80) - diethyl ether(50:50)