Реакция #2146761

ord-2ea8ceb3eb0d4f57b57f39fb5e7da474

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияFor workup, the precipitate was filtered off
  2. 2
    Промывкаwashed with dichloromethane
  3. 3
    ПромывкаThe filtrate was washed twice with NaHCO3-solution
  4. 4
    ДругоеThe layers were separated
  5. 5
    Экстракцияthe aqueous phase was extracted twice with dichloromethane
  6. 6
    СушкаThe organic phases were dried with MgSO4
  7. 7
    Другоеevaporated

Методика

25 g (137.7 mmol) of 7-Chloro-6-fluoro-isoquinoline (3) were in dissolved in 500 ml of dichloromethane. At room temperature 50.9 g (206.5 mmol) of 3-Chloro-benzene-carboperoxoic acid (70%) were added and the mixture was stirred at room temperature until complete conversion is achieved. For workup, the precipitate was filtered off and washed with dichloromethane. The filtrate was washed twice with NaHCO3-solution. The layers were separated and the aqueous phase was extracted twice with dichloromethane. The organic phases were dried with MgSO4 and evaporated. The so obtained solid material (18.4 g) was used without further purification. Rt=0.87 min (Method C). Detected mass: 198.1/200.1 (M+H+).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08278294B2uspto-grants-2012_10