HRID1461118

反应详情

EQUATION

反应方程式

HRID 1461118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (benzoyloxy)acetyl chloride (1.98 g, 0.01 mole), pyrrolidone (0.85 g, 0.01 mole) and pyridine (0.8 g, 0.01 mole) in acetone (10 ml) was refluxed for 3 h. The cooled mixture was filtered and evaporated in vacuo. The residue was dissolved in ethyl acetate (50 ml) and the solution washed with a 2% aqueous solution of sodium bicarbonate, 2M hydrochloric acid and water. After drying over anhydrous sulphate, the organic phase was evaporated under reduced pressure to give a residue which crystallized by addition of ether. Recrystallization from ether-petroleum ether yielded 1.6 g (65%) of the title compound. Mp 83°-84° C.

WORKUP

后处理

  1. temperaturewas refluxed for 3 h
  2. filtrationThe cooled mixture was filtered
  3. customevaporated in vacuo
  4. dissolutionThe residue was dissolved in ethyl acetate (50 ml)
  5. washthe solution washed with a 2% aqueous solution of sodium bicarbonate, 2M hydrochloric acid and water
  6. dry with materialAfter drying over anhydrous sulphate
  7. customthe organic phase was evaporated under reduced pressure
  8. customto give a residue which
  9. customcrystallized by addition of ether
  10. customRecrystallization from ether-petroleum ether