Water → 1-Dimethylsulfamoyl-2-ethylimidazole

HRID 1655136

反応式

HRID 1655136 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 to the reaction mixture after which the organic layer is separated and concentrated. The residue is dissolved in ethyl acetate (1 liter) and washed with water, and then dried over sodium sulfate and concentrated. Distillation gives 1-dimethylsulfamoyl-2 -ethylimidazole (182 g) as a colorless liquid.

後処理

  1. customis separated
  2. concentrationconcentrated
  3. dissolutionThe residue is dissolved in ethyl acetate (1 liter)
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. distillationDistillation

出典と根拠

ORDレコード
ord-266522fce9ce4785a5f23b6ab5a6afdb
出典データセット
uspto-grants-1995_04
特許番号
US05409936

関連ノート

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