Реакция #1722224

ord-554a3ee4d6544b24b4d89cd8fe608e5d

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted with ethyl acetate (3×150 mL)
  2. 2
    ПромывкаThe combined organic extracts were washed with brine (2×100 mL)
  3. 3
    Сушкаdried with magnesium sulfate
  4. 4
    Фильтрацияfiltered
  5. 5
    Другоеevaporated in vacuo
  6. 6
    ДругоеThe residue was purified on a silica gel column
  7. 7
    Промывкаeluted with 25% ethyl acetate in dichloromethane
  8. 8
    ДругоеThe product (I1) was isolated 0.48 g (46%) as a light orange solid

Методика

To the benzoxazinone (I6) (1.38 g, 4.17 mmol) in DMF (5 mL) was added potassium carbonate (1.40 g, 10.1 mmol), and the solution was stirred at room temperature for 1 hour. The solution was diluted with water and extracted with ethyl acetate (3×150 mL). The combined organic extracts were washed with brine (2×100 mL), dried with magnesium sulfate filtered, and evaporated in vacuo. The residue was purified on a silica gel column eluted with 25% ethyl acetate in dichloromethane. The product (I1) was isolated 0.48 g (46%) as a light orange solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06509335B1uspto-grants-2003_01