HRID1649326
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
- 120 °C
PROCEDURE
实验过程
A mixture of 2-oxazolidinone (9.0 g, 0.10 mole) and 25 ml (0.18 mole) of ethyl trichloroacetate were heated to 120° C. in an oil bath. A small amount (ca 50 mg) of 4-dimethylaminopyridine was added to the stirred solution, during which time vigorous reflux began. After removing most of the chloroform by a Dean-Stark trap, the dark solution was allowed to cool to room temperature. Bulb to bulb distillation at 105° C.-120° C. (0.05 mm) yielded 14.1 g (0.0887 mole, 89 percent yield) of the product as a clear liquid which solidified to a colorless solid (mp 40° C.-44° C.) on standing at room temperature. Spectral data confirmed its structure.
WORKUP
后处理
- temperaturevigorous reflux
- customAfter removing most of the chloroform by a Dean-Stark trap
- temperatureto cool to room temperature
- distillationBulb to bulb distillation at 105° C.-120° C. (0.05 mm)