HRID1795731

反应详情

EQUATION

反应方程式

HRID 1795731 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 118 g of 4-methyl-1,4-pentanediol, 111 g of triethylamine and 400 ml of toluene at 20° C., 157 g of 5-norbornene-2-carbonyl chloride was added over one hour. After 5 hours of stirring, 200 ml of water was added to the reaction solution to stop the reaction whereupon the mixture separated. The organic layer was washed with water and saturated sodium chloride water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was purified by vacuum distillation, collecting 214 g of 0.4-hydroxy-4-methylpentyl 5-norbornene-2-carboxylate (boiling point: 111–113° C./27 Pa, yield: 90%).

WORKUP

后处理

  1. customthe reaction whereupon the mixture
  2. customseparated
  3. washThe organic layer was washed with water and saturated sodium chloride water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuum
  6. distillationIt was purified by vacuum distillation
  7. customcollecting 214 g of 0