Reaktion #413651

ord-a39ea9eac1b64affa0731f5f0d09ece4

Reaktionsgleichung

O
Water
CCc1ncc[nH]1
2-ethylimidazole
CCN(CC)CC
triethylamine
CN(C)S(=O)(=O)Cl
dimethylsulfamoyl chloride
CCc1nccn1S(=O)(=O)N(C)C
1-dimethylsulfamoyl-2-ethylimidazole
Ausbeute 86.1%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe organic layer is separated
  2. 2
    Einengenconcentrated
  3. 3
    workup.DISSOLUTIONThe residue is dissolved in ethyl acetate (1 liter)
  4. 4
    Waschenwashed with water
  5. 5
    TrocknenThe solution is dried over sodium sulfate
  6. 6
    Einengenconcentrated
  7. 7
    workup.DISTILLATIONDistillation

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05268377uspto-grants-1993_12