Water → 1-Dimethylsulfamoyl-2-ethylimidazole

HRID 326469

反応式

HRID 326469 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 661302-EthylimidazoleHCID 83372Dimethylsulphamoyl chloride

生成物 1

HCID 232931831-Dimethylsulfamoyl-2-ethylimidazole収率 86.1%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a39ea9eac1b64affa0731f5f0d09ece4
出典データセット
uspto-grants-1993_12
特許番号
US05268377

関連ノート

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