Реакция #933795

ord-6d7d148d343648b0a8fd0c8b95b45100

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated
  2. 2
    ТемператураThe mixture was then heated
  3. 3
    Температураunder reflux for a further 2 hours
  4. 4
    Температураcooled
  5. 5
    Другоеthe organic phase was separated
  6. 6
    Сушкаdried over sodium sulfate
  7. 7
    ДругоеAfter removing the solvent under reduced pressure
  8. 8
    Другоеthe solid residue was recrystallized from methylcyclohexane

Методика

20.6 g (83 mmol) of 1-(3,5-di-tert.-butyl-4-hydroxy-phenyl)ethanone were dissolved in 50 ml of methylene chloride with stirring and heated to boiling, and 14.4 g (90 mmol) of bromine were added dropwise in the course of 15 minutes. The mixture was then heated under reflux for a further 2 hours and cooled, 50 ml of water were added, and the organic phase was separated and dried over sodium sulfate. After removing the solvent under reduced pressure, the solid residue was recrystallized from methylcyclohexane.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05137897uspto-grants-1992_08