Реакция #48418

ord-87541fac1f3341f8b17e1ec1523c152f

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe reaction was quenched with aqueous sodium sulfite solution
  2. 2
    Экстракцияthe mixture was extracted with ethyl acetate
  3. 3
    ПромывкаThe organic layer was washed with saturated aqueous sodium carbonate (3×), saturated brine
  4. 4
    Сушкаdried over magnesium sulfate
  5. 5
    Фильтрацияfiltered
  6. 6
    Концентрированиеconcentrated

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07745427B2uspto-grants-2010_06