HRID1835965
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 4-hydroxy-4-methylpentyl 5-norbornene-2-carboxylate (boiling point: 111-113° C./27 Pa, yield: 90%).
WORKUP
后处理
- customthe reaction whereupon the mixture
- customseparated
- washThe organic layer was washed with water and saturated sodium chloride water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuum
- distillationIt was purified by vacuum distillation