Реакция #156246

ord-ac7601b9049e41ac8c10308a8a2b2789

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwhile heated
  2. 2
    Температураunder reflux
  3. 3
    Экстракцияfollowed by extraction by ethyl acetate
  4. 4
    СушкаThe organic layer was dried by anhydrous sodium sulfate, and condensed under reduced pressure
  5. 5
    ДругоеThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=85:15)
  6. 6
    Другоеcondensed under reduced pressure
  7. 7
    Другоеthe residue was recrystallized from ether/hexane

Методика

7-[3-(2,3-Dioxo-2,3-dihydroindol-1-yl)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.3 g) was suspended in hydrazine hydrate (3 ml), and the liquid was stirred for two hours while heated under reflux. The reaction mixture was cooled to room temperature. Water was added thereto, followed by extraction by ethyl acetate. The organic layer was dried by anhydrous sodium sulfate, and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=85:15). The purified product was condensed under reduced pressure, and the residue was recrystallized from ether/hexane, thereby obtaining the title compound (0.18 g) as a pale brownish white powder.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822453B2uspto-grants-2014_09