HRID267980

反应详情

EQUATION

反应方程式

HRID 267980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 15 g (0.033 mole) of 4'-fluoro-5-[4-(α-hydroxy-α-phenylbenzyl)piperidino]valerophenone hydrochloride and 15 g of hydroxylamine hydrochloride in 120 ml of pyridine is stirred on a steam bath for about 4 hours then cooled to room temperature. The pyridine is removed at reduced pressure on a steam bath, and the residue is triturated with a dilute sodium hydroxide solution and extracted with chloroform. The chloroform extract is washed with water, dried over magnesium sulfate, filtered and concentrated to a residue which is triturated with hexane. The resulting solid is filtered off and recrystallized from ethanol to give 4'-fluoro-5-[4-(α-hydroxy-α-phenylbenzyl)piperidino]valerophenone oxime.

WORKUP

后处理

  1. customThe pyridine is removed at reduced pressure on a steam bath
  2. customthe residue is triturated with a dilute sodium hydroxide solution
  3. extractionextracted with chloroform
  4. extractionThe chloroform extract
  5. washis washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated to a residue which
  9. customis triturated with hexane
  10. filtrationThe resulting solid is filtered off
  11. customrecrystallized from ethanol