HRID231269

反应详情

EQUATION

反应方程式

HRID 231269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 70 ml of tetrahydrofuran is suspended 0.86 g of sodium hydride, to which a solution of 10.2 g of 1-benzyl-3-(12-cyclohexyldodecyl)glycerine in 50 ml of tetrahydrofuran is added dropwise at room temperature with stirring. After 40 minutes stirring at room temperature, 5.11 g of methyl iodide is added and the mixture is further stirred for 2 hours. The solvent is then distilled off under reduced pressure and the residue is extracted with hexane. The extract layer is washed with water, dried and concentrated to obtain crude 1-benzyl-2-methyl-3-(12cyclohexyldodecyl)glycerine which in turn is dissolved in a mixed solvent consisting of 100 ml of ethanol and 30 ml of acetic acid. The solution is shaked in the presence of 10% palladium-carbon under hydrogen streams. The catalyst is removed by filtration and the filtrate is concentrated to obtain 9.6 g of the captioned compound as a crude product.

WORKUP

后处理

  1. stirringAfter 40 minutes stirring at room temperature
  2. stirringthe mixture is further stirred for 2 hours
  3. distillationThe solvent is then distilled off under reduced pressure
  4. extractionthe residue is extracted with hexane
  5. washThe extract layer is washed with water
  6. customdried
  7. concentrationconcentrated