HRID1709893

反应详情

EQUATION

反应方程式

HRID 1709893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound was prepared according to the procedure used to synthesize the compound of Example 1. A mixture of 3.0 g (0.01 mole) of [α,α-bis(p-fluorophenyl)]-4-piperidinemethanol, 2.4 g (0.01 mole) of 1-[4-(3-chloropropoxy)-2-methoxyphenyl]ethanone, 5.3 g (0.05 mole) of anhydrous sodium carbonate and 0.3 g of potassium iodide in 100 ml of 1-butanol gave a gum as residue. The gum was purified by column chromatography on 80 g of Florisil® and the fractions eluted with 20% acetone in benzene were combined and concentrated under reduced pressure to give a solid as residue. The solid was converted to the hydrochloride and this solid was recrystallized from 2-propanol-isopropyl ether to yield 2.2 g (40%) of white power, m.p. 196°-197° C.

WORKUP

后处理

  1. customThis compound was prepared
  2. customgave a gum as residue
  3. customThe gum was purified by column chromatography on 80 g of Florisil®
  4. washthe fractions eluted with 20% acetone in benzene
  5. concentrationconcentrated under reduced pressure
  6. customto give a solid as residue
  7. customthis solid was recrystallized from 2-propanol-isopropyl ether
  8. customto yield 2.2 g (40%) of white power, m.p. 196°-197° C.