반응 #63526

ord-ae6f718601e841f48812a2ddf7849e44

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    workup.ADDITIONThe reaction mixture is poured onto ice-water
  3. 3
    추출extracted with ether
  4. 4
    세척The ether layer is washed with an aqueous sodium hydrogen carbonate solution
  5. 5
    건조an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONAfter distilling off the solvent
  7. 7
    workup.DISTILLATIONthe resulting residue is distilled under reduced pressure

실험 절차

N-Ethyl-cyclohexylamine (2.6 g) is dissolved in dry benzene (20 ml). To the solution are added dropwise with stirring chloroacetyl chloride (2.6 g) and triethylamine (2.4 g) under ice-cooling. The mixture is stirred under ice-cooling for one hour and further at room temperature for one hour. The reaction mixture is poured onto ice-water and extracted with ether. The ether layer is washed with an aqueous sodium hydrogen carbonate solution and an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After distilling off the solvent, the resulting residue is distilled under reduced pressure to give N-ethyl-N-cyclohexyl-chloroacetamide (3 g), b.p. 118°-120° C./0.2 mmHg.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04766120uspto-grants-1988_08