1,2-Dichloroethane → 3-(2-Chloroethyl)-5,5-dimethylimidazolidine-2,4-dione

HRID 268027

반응식

HRID 268027 반응식
[CH3:1][C:2]1([CH3:9])[NH:6][C:5](=[O:7])[NH:4][C:3]1=[O:8].C(=O)([O-])[O-].[K+].[K+].[Cl:16][CH2:17][CH2:18]Cl>CN(C)C=O>[Cl:16][CH2:17][CH2:18][N:4]1[C:3](=[O:8])[C:2]([CH3:9])([CH3:1])[NH:6][C:5]1=[O:7]

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 6491DimethylhydantoinHCID 11430Potassium Carbonate

생성물 1

HCID 2980853-(2-Chloroethyl)-5,5-dimethylimidazolidine-2,4-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  1. customis reacted for 18 hours and 20 minutes at 90°C to 100°C internal temperature (external temperature 155°C)
  2. customwhilst constantly removing
  3. customthe resulting water of reaction
  4. distillationby azeotropic circulatory distillation
  5. customWater of reaction
  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 under a waterpump vacuum
  9. customthe residue is dried to constant weight at 100°C

출처 및 근거

ORD 기록
ord-cdd7c2dea73644fc9748ec2a52c2a368
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03946034

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