HRID1709898

反应详情

EQUATION

反应方程式

HRID 1709898 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, 1.9 g (0.01 mole) of 1-chloro-3-(4-fluorophenoxy) propane, 5.3 g (0.035 mole) of anhydrous sodium carbonate and 0.3 g of potassium iodide in 100 ml of 1-butanol gave a solid as residue. The solid was further purified by column chromatography on 60 g of Florisil®. Fractions eluted with 2-10% acetone in benzene were combined and concentrated to give a solid residue. The solid was converted to the furmaric acid salt and this solid was recrystallized from isopropanol to yield 2.2 g (39%) of title compound as a white solid, mp 155°-157° C.

WORKUP

后处理

  1. customThis compound was prepared
  2. customgave a solid as residue
  3. customThe solid was further purified by column chromatography on 60 g of Florisil®
  4. washFractions eluted with 2-10% acetone in benzene
  5. concentrationconcentrated
  6. customto give a solid residue
  7. customthis solid was recrystallized from isopropanol