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 1,485 ml of dimethylformamide is reacted for 18 hours and 20 minutes at 90° C to 100° C internal temperature (external temperature 155° C), the water of reaction produced being removed continuously by azeotropic circulatory distillation. Water of reaction split off: 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 in a water pump 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)
- customproduced
- custombeing removed continuously by azeotropic circulatory distillation
- customWater of reaction
- customsplit off
- 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 in a water pump vacuum
- customthe residue is dried to constant weight at 100° C