HRID231268

反应详情

EQUATION

反应方程式

HRID 231268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In 100 ml of dimethylsulfoxide is suspended 1.4 g of sodium hydride, to which 9.73 g of benzyl alcohol is added dropwise at room temperature with stirring. After the addition is over, the mixture is gradually heated to 60° C. and stirred at that temperature for 40 minutes. Then, a solution of 9.7 g of 1,2-epoxy-3-(12-cyclohexyldodecyloxy)propane in 50 ml of tetrahydrofuran is added dropwise to the mixture and the resulting mixture is stirred at 60° C. for 2 hours. The thus obtaind reaction mixture is then neutralized with dilute hydrochloric acid and extracted with hexane-ethyl acetate (1:1). The extract layer is washed with water, dried and concentrated. The residue is purified by silica gel column chromatography to yield 10.2 g of the captioned compound as an oily substance.

WORKUP

后处理

  1. additionAfter the addition
  2. stirringstirred at that temperature for 40 minutes
  3. stirringthe resulting mixture is stirred at 60° C. for 2 hours
  4. customThe thus obtaind reaction mixture
  5. extractionextracted with hexane-ethyl acetate (1:1)
  6. washThe extract layer is washed with water
  7. customdried
  8. concentrationconcentrated
  9. customThe residue is purified by silica gel column chromatography