HRID2071591

反应详情

EQUATION

反应方程式

HRID 2071591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customis reacted for 18 hours and 20 minutes at 90° C to 100° C internal temperature (external temperature 155° C)
  2. customproduced
  3. custombeing removed continuously by azeotropic circulatory distillation
  4. customWater of reaction
  5. customsplit off
  6. customThereafter, the reaction mixture, whilst still hot, is separated by filtration from the potassium chloride
  7. customproduced
  8. concentrationthe filtrate is concentrated on a rotary evaporator at 100° C in a water pump vacuum
  9. customthe residue is dried to constant weight at 100° C