反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe pyridine is removed at reduced pressure on a steam bath
- customthe residue is triturated with a dilute sodium hydroxide solution
- extractionextracted with chloroform
- extractionThe chloroform extract
- washis washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated to a residue which
- customis triturated with hexane
- filtrationThe resulting solid is filtered off
- customrecrystallized from ethanol