Реакция #491900

ord-27a094df04064df4bb8682d15163dd9a

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONpoured carefully on ice with mechanical stirring
  2. 2
    ЭкстракцияThe aqueous solution was extracted three times with dichloromethane
  3. 3
    СушкаThe combined organic layers were dried over magnesium sulfate
  4. 4
    Другоеevaporated

Методика

53.0 g (236, mmol) of 6-bromo-isoquinoline 2-oxide (4) were heated in 400 ml of POCl3 under reflux conditions in two portions. After 4 h, the reaction was cooled to room temperature and poured carefully on ice with mechanical stirring. The aqueous solution was extracted three times with dichloromethane. The combined organic layers were dried over magnesium sulfate and evaporated, which gave 42.8 g of the title compound, which was used without further purification. Rt=1.64 min (Method C). Detected mass: 242.1/244.2 (M+H+).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08748614B2uspto-grants-2014_06