HRID386327

反应详情

EQUATION

反应方程式

HRID 386327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of sodium acrylate (2.5 g, 13.4 mmol), 4′-propyl-bicyclohexyl-4-carboxylic acid 3-bromo-propyl ester (synthesis described for preferred example 1) (5.0 g, 13.4 mmol) and sodium iodide (2.5 g, 16.7 mmol) in dimethylformamide (150 ml) is stirred at 130° C. overnight. The mixture is cooled to room temperature, poured into water, and this is extracted twice with diethyl ether. The ethereal solution is washed with water and then dried over sodium sulphate. The solution is evaporated to dryness and purified by flash column chromatography using DCM/petrol (1/1) as eluant to give upon evaporation of the appropriate fractions a colourless oil.

WORKUP

后处理

  1. temperatureThe mixture is cooled to room temperature
  2. extractionthis is extracted twice with diethyl ether
  3. washThe ethereal solution is washed with water
  4. dry with materialdried over sodium sulphate
  5. customThe solution is evaporated to dryness
  6. custompurified by flash column chromatography
  7. customto give upon evaporation of the appropriate fractions a colourless oil