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
CONDITIONS
反应条件
- 温度
- 157 °C
PROCEDURE
实验过程
The crude isoamyl glycidyl ether (140 g), water (140 g; 7.78 mol), lauric acid (7.64 g; 0.038 mol) and potassium hydroxide (2.14 g; 0.038 mol) were placed in a 2-l autoclave, and the mixture was heated up to 157° C. while stirring it. The mixture was stirred for 5 hours as it was, and was then allowed to cool down to room temperature. The mixture was extracted with ethyl acetate (500 ml), and the extract was washed twice with water (300 ml). The solvent was then distilled off to obtain 157 g of crude monoisoamyl glyceryl ether. This crude product was purified by vacuum distillation (2 mmHg, 114-115° C.) to obtain 103 g of monoisoamyl glyceryl ether as a colorless transparent oil (total yield: 71%). Quenching of a proton signal (methylene in an epoxy ring) at δ=2.60, 2.80 was observed by 1H-NMR (200 MHz), thereby identifying the compound. The purity of the compound was found to be at least 99% by GLC.
WORKUP
后处理
- stirringThe mixture was stirred for 5 hours as it
- temperatureto cool down to room temperature
- extractionThe mixture was extracted with ethyl acetate (500 ml)
- washthe extract was washed twice with water (300 ml)
- distillationThe solvent was then distilled off