Реакция #1246187

ord-d5e9690b5efa4d97bc82464d6124b039

Реагенты

Нет

Растворители

Условия реакции

Температура
150°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеby irradiating microwaves
  2. 2
    Другоеterminated
  3. 3
    Другоеthe reaction
  4. 4
    Промывкаwashed with water
  5. 5
    СушкаThe organic layer was dried over anhydrous magnesium sulfate
  6. 6
    Концентрированиеconcentrated
  7. 7
    Другоеvacuum evaporation
  8. 8
    ДругоеThe residue was re-crystallized in dichloromethane

Методика

2′,6′-Difluoroacetophenone (0.468 g, 3 mmol) was dissolved in anhydrous hydrazine (2 ml), followed by irradiating microwaves thereon with stirring at 150° C. for 5 min. The addition of water (0.5 ml) at 0° C. terminated the reaction. Afterwards, the reaction solution was diluted with ethyl acetate (10 ml) and washed with water. The organic layer was dried over anhydrous magnesium sulfate and concentrated using vacuum evaporation. The residue was re-crystallized in dichloromethane to give the title compound (Yield 85%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07812045B2uspto-grants-2010_10