HRID2290809

反应详情

EQUATION

反应方程式

HRID 2290809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2.16 g of benzyl alcohol and 30 ml of dimethylformamide was added 1.2 g of oily sodium hydride (60%). After stirring the mixture for 30 minutes at 20° to 25° C., 10 g of 1,12-dibromododecane was added to the mixture in one portion followed by stirring for 2 hours at 25° to 30° C. After the reaction was over, 300 ml of water was added to the reaction mixture and the product was extracted with n-hexane. The extract was washed with water, dried over anhydrous magnesium sulfate, and then, the solvent was distilled off. The oily residue was applied to silica gel column chromatography and eluted with a mixture of n-hexane and ether (9:1) to provide 3.8 g of 12-benzyloxy-1-bromododecane as an oily product.

WORKUP

后处理

  1. stirringby stirring for 2 hours at 25° to 30° C
  2. additionwas added to the reaction mixture
  3. extractionthe product was extracted with n-hexane
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off
  7. washeluted with a mixture of n-hexane and ether (9:1)