HRID26906

反应详情

EQUATION

反应方程式

HRID 26906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.2 g. of 3-(2',4'-difluoro-4-biphenylyl)-3-hydroxybutyric acid ethyl ester in 10 ml. of dichloromethane is saturated with dry HCl gas and 1 ml. of SOCl2 is added. The mixture is warmed to 50° for 2 hours and solvent is removed. The residue, 3'(2',4'-difluoro-4-biphenylyl)-3-chlorobutyric acid ethyl ester, is dissolved in 100 ml. of methanol and hydrogenated on 100 mg. of platinum oxide under normal pressure at 25°. The precipitate is filtered off. A solution of 0.4 g. of NaOH in 5 ml. of water is added to the filtrate. The mixture is heated under reflux for 2 hours and evaporated and the residue is dissolved in water and worked up in the customary manner to give 3-(2',4'-difluoro-4-biphenylyl)butyric acid, m.p. 109°-110°.

WORKUP

后处理

  1. temperatureThe mixture is warmed to 50° for 2 hours
  2. customsolvent is removed
  3. dissolutionThe residue, 3'(2',4'-difluoro-4-biphenylyl)-3-chlorobutyric acid ethyl ester, is dissolved in 100 ml
  4. customat 25°
  5. filtrationThe precipitate is filtered off
  6. additionof water is added to the filtrate
  7. temperatureThe mixture is heated
  8. temperatureunder reflux for 2 hours
  9. customevaporated
  10. dissolutionthe residue is dissolved in water