Reaktion #50160

ord-61bc5d6024df4362ad3eac19e9288450

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
    Sonstigeis separated
  2. 2
    Einengenconcentrated
  3. 3
    workup.DISSOLUTIONThe residue is dissolved in ethyl acetate (1 liter)
  4. 4
    Waschenwashed with water
  5. 5
    Trocknendried 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 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424316uspto-grants-1995_06