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
A mixture of 1,664 g of 5,5-dimethyl-hydantoin (13.0 mols), 897 g of anhydrous potassium carbonate (6.5 mols), 5,148 g of 1,2-dichloroethane (52 mols) and 1,458 ml of dimethylformamide is reacted for 18 hours and 20 minutes at 90°C to 100°C internal temperature (external temperature 155°C), whilst constantly removing the resulting water of reaction by azeotropic circulatory distillation. Water of reaction eliminated: 110 g (94.0% of theory). Thereafter the reaction mixture, whilst still hot, is separated by filtration from the potassium chloride produced, the filtrate is concentrated on a rotary evaporator at 100°C under a waterpump vacuum and the residue is dried to constant weight at 100°C and 10-1 mm Hg.
WORKUP
后处理
- customis reacted for 18 hours and 20 minutes at 90°C to 100°C internal temperature (external temperature 155°C)
- customwhilst constantly removing
- customthe resulting water of reaction
- distillationby azeotropic circulatory distillation
- customWater of reaction
- customThereafter the reaction mixture, whilst still hot, is separated by filtration from the potassium chloride
- customproduced
- concentrationthe filtrate is concentrated on a rotary evaporator at 100°C under a waterpump vacuum
- customthe residue is dried to constant weight at 100°C