반응 #76622

ord-90dbca10add4400988721a2a9294db4f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with diethyl ether
  2. 2
    세척The organic phase was washed twice with water
  3. 3
    건조dried over magnesium sulphate
  4. 4
    기타evaporated to dryness
  5. 5
    기타the residue chromatographed on silica gel
  6. 6
    세척for the elution

실험 절차

2.05 g (7.59 mmol) of 2′-acetyl-2-bromo-N-methylacetanilide and 2 g (30.77 mmol) of sodium azide were stirred in 20 ml of dimethylformamide at room temperature for 4 hours. The resulting mixture was diluted with water and extracted with diethyl ether. The organic phase was washed twice with water, dried over magnesium sulphate, evaporated to dryness and the residue chromatographed on silica gel using ethyl acetate/petrol 5:3 for the elution. There was obtained 910 mg of 2′-acetyl-2-azido-N-methylacetanilide as a colorless gum. MS: m/e 233 [M+H]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06703387B2uspto-grants-2004_03