HRID1193675

反应详情

EQUATION

反应方程式

HRID 1193675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 5.51 g (0.019 mole) of 4-[bis(4-fluorophenyl)methyl]piperidine, 4.42 g (0.019 mole) of 1-(3-chloropropoxy)-3,5-dimethoxybenzene and potassium carbonate (5.53 g, 0.04 mole) was heated overnight at reflux in 350 ml of 1-butanol containing potassium iodide (0.3 g). The reaction mixture was stripped to dryness and the residue partitioned between chloroform-5% sodium hydroxide and chloroform-water. Removal of chloroform gave a brown oil. The oil was subjected to chromatography on a silica gel column using a gradient elution series of hexane-ethyl acetate and ethyl acetate-dimethoxyethane. After combining proper fractions eluted from the column and removing solvent, the residual oil was dried in vacuo overnight at 80° C. This produced 2.61 g (28.5%) of brown oil.

WORKUP

后处理

  1. temperaturewas heated overnight
  2. customthe residue partitioned between chloroform-5% sodium hydroxide and chloroform-water
  3. customRemoval of chloroform
  4. customgave a brown oil
  5. washeluted from the column
  6. customremoving solvent
  7. customthe residual oil was dried in vacuo overnight at 80° C