Water → 1-Dimethylsulfamoyl-2-ethylimidazole

HRID 326469

반응식

HRID 326469 반응식
[CH2:1]([C:3]1[NH:4][CH:5]=[CH:6][N:7]=1)[CH3:2].C(N(CC)CC)C.[CH3:15][N:16]([CH3:21])[S:17](Cl)(=[O:19])=[O:18].O>C(Cl)(Cl)Cl>[CH3:15][N:16]([CH3:21])[S:17]([N:4]1[CH:5]=[CH:6][N:7]=[C:3]1[CH2:1][CH3:2])(=[O:19])=[O:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 661302-EthylimidazoleHCID 83372Dimethylsulphamoyl chloride

생성물 1

HCID 232931831-Dimethylsulfamoyl-2-ethylimidazole수율 86.1%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a stirred solution of 2-ethylimidazole (100 g) and triethylamine (115 g) in chloroform (800 ml) at 0° C. is added a solution of dimethylsulfamoyl chloride (153 g) in chloroform (200 ml). The mixture is stirred overnight at room temperature. Water (1.5 liter) is added thereto and the organic layer is separated therefrom and concentrated. The residue is dissolved in ethyl acetate (1 liter) and washed with water. The solution is dried over sodium sulfate and concentrated. Distillation gives 1-dimethylsulfamoyl-2-ethylimidazole (182 g) as colorless liquid.

후처리

  1. customthe organic layer is separated
  2. concentrationconcentrated
  3. dissolutionThe residue is dissolved in ethyl acetate (1 liter)
  4. washwashed with water
  5. dry with materialThe solution is dried over sodium sulfate
  6. concentrationconcentrated
  7. distillationDistillation

출처 및 근거

ORD 기록
ord-a39ea9eac1b64affa0731f5f0d09ece4
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05268377

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