HRID1608029

反应详情

EQUATION

反应方程式

HRID 1608029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of 2.12 g (20 mmol) of 2-methoxy-1,3-propanediol 7.99 g (24 mmol) of octadecyl bromide, 2.43 g (30 mmol) of potassium cyanate and 1.29 g (4 mmol) of tetrabutyl ammonium bromide in 100 ml of dry acetonitrile was refluxed with stirring, at 100° C. for 24 hours. The resultant mixture was then diluted with hot methylene chloride, filtered and the filtrate concentrated in vacuo. The crude product was then purified by flash silica gel chromatography employing a mixture of petroleum ether and ethyl acetate in a 4:1 ratio as the eluent to yield the title compound as a solid, m.p. 56°-58° C.

WORKUP

后处理

  1. temperaturewas refluxed
  2. filtrationfiltered
  3. concentrationthe filtrate concentrated in vacuo
  4. customThe crude product was then purified by flash silica gel chromatography
  5. additiona mixture of petroleum ether and ethyl acetate in a 4:1 ratio as the eluent