반응 #48418

ord-87541fac1f3341f8b17e1ec1523c152f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the reaction was quenched with aqueous sodium sulfite solution
  2. 2
    추출the mixture was extracted with ethyl acetate
  3. 3
    세척The organic layer was washed with saturated aqueous sodium carbonate (3×), saturated brine
  4. 4
    건조dried over magnesium sulfate
  5. 5
    여과filtered
  6. 6
    농축concentrated

실험 절차

Oxone® ((16.1 mg, 0.11 mmol) was added to a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-1-[2-(methylthio)ethyl]-2-oxoazepan-3-ylcarbamate (22 mg, 0.053 mmol) in methanol (2 mL) and water (2 mL). After 6 h excess oxone (32 mg, 0.22 mmol) was added. After 18 h, the reaction was quenched with aqueous sodium sulfite solution and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium carbonate (3×), saturated brine, dried over magnesium sulfate, filtered and concentrated to give the title compound. MS 447 (M+1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745427B2uspto-grants-2010_06