HRID1902834

反应详情

EQUATION

反应方程式

HRID 1902834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 11.1 g (0.05 mole) of 4-(p-fluorobenzoyl)-4-hydroxy-piperidine, 14.6 g (0.06 mole) of 3-(p-acetyl-o-methoxyphenoxy)-propyl chloride and 25 g of anhydrous sodium carbonate in 350 ml iso-butylacetate was allowed to reflux for 48 h. The mixture was filtered and the filtrate was concentrated under vacuum. The residual oil was converted to the HCl salt. 1-[3-(p-Acetyl-o-methoxyphenoxy)propyl]-4-(p-fluorobenzoyl)-4-hydroxy-piperidine hydrochloride was recrystallised from ethanol. Melting point 160°-162° C. Yield 16.2 g. Said product contained a certain amount of ethanol which can only be removed by extreme means.

WORKUP

后处理

  1. temperatureto reflux for 48 h
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated under vacuum
  4. custom1-[3-(p-Acetyl-o-methoxyphenoxy)propyl]-4-(p-fluorobenzoyl)-4-hydroxy-piperidine hydrochloride was recrystallised from ethanol
  5. customcan only be removed by extreme means