HRID1709897

反应详情

EQUATION

反应方程式

HRID 1709897 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, 1.8 g (0.01 mole) of 1-chloro-3-(4-methylphenoxy) 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 gum as residue. The gum was purified by column chromatography on 100 g of Florisil®. Fractions eluted with 10% acetone in benzene were combined and concentrated to give a gum. This gum was converted to the fumaric acid salt and the solid was recrystallized from absolute ethanol to yield 3.2 g (56%) of title compound as a white solid, mp 193°-194° C. with decomposition. pe f 49495948.hsc

WORKUP

后处理

  1. customThis compound was prepared
  2. customgave a gum as residue
  3. customThe gum was purified by column chromatography on 100 g of Florisil®
  4. washFractions eluted with 10% acetone in benzene
  5. concentrationconcentrated
  6. customto give a gum
  7. customthe solid was recrystallized from absolute ethanol