HRID2397403

反应详情

EQUATION

反应方程式

HRID 2397403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9 gm (0.03 mol) of ethyl 4-(2'-fluoro-4-biphenylyl)-4-oxo-butyrate, 150 ml of absolute isopropanol and 6.2 gm (0.03 mol) of freshly distilled aluminum isopropylate was refluxed on a boiling water bath, while condensing the vapors in a descending condenser, until no more acetone was detectable in the distillate. After removing the solvent in vacuo, the residue was covered with ether, the mixture was acidified with dilute hydrochloric acid, and the ethereal phase was separated, washed with sodium bicarbonate and water. After distilling off the solvent, the solid residue was recrystallized from cyclohexane, to yield 6 gm (78% of theory) of colorless γ-(2'-fluoro-4-biphenylyl)-γ-butyrolactone, m.p. 74°-75° C.

WORKUP

后处理

  1. temperaturewas refluxed on a boiling water bath, while condensing the vapors in a descending condenser
  2. customAfter removing the solvent in vacuo
  3. customthe ethereal phase was separated
  4. washwashed with sodium bicarbonate and water
  5. distillationAfter distilling off the solvent
  6. customthe solid residue was recrystallized from cyclohexane