Реакция #321457

ord-2eee10b31a814b8794957221e196d060

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеCatalytic hydrogenation decomposition reaction
  2. 2
    ДругоеAfter the completion of the reaction
  3. 3
    Фильтрацияthe catalyst was filtered
  4. 4
    Концентрированиеthe filtrate was concentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in isopropyl ether
  6. 6
    Промывкаwashed with water
  7. 7
    Другоеdried
  8. 8
    workup.DISTILLATIONthe solvent was distilled off
  9. 9
    ДругоеThe residue was crystallized from methanol

Методика

Triethylamine (5.0 ml, 35.6 mmol) was added to a solution of 5-bromo-2-bromomethyl-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran (12.4 g, 35.6 mmol) in ethanol (100 ml). Catalytic hydrogenation decomposition reaction was carried out on 5% palladium carbon under a hydrogen atmosphere. After the completion of the reaction, the catalyst was filtered and the filtrate was concentrated. The residue was dissolved in isopropyl ether, washed with water, dried and the solvent was distilled off. The residue was crystallized from methanol to obtain the desired compound (8.84 g, yield: 92.2%), m.p. 39°-40° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05594154uspto-grants-1997_01