Реакция #7935

ord-3e877446746d40fd8d3411e8cf355c24

Растворители

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated at 60° C. for two hours
  2. 2
    Температураcooled to room temperature
  3. 3
    Другоеevaporated under vacuum
  4. 4
    Другоеto leave a yellow semi-solid
  5. 5
    Промывкаwashed with water and brine
  6. 6
    Сушкаdried over MgSO4
  7. 7
    Фильтрацияfiltered
  8. 8
    Другоеevaporated under vacuum

Методика

A suspension of 9a-butyl-7-methoxy-4-(4-methoxymethoxy-phenyl)-1,2,9,9a-tetrahydro-3H-fluoren-3-one (813 mg, 2 mmol) in methanol (12 mL) was warmed in an oil bath at 60° C. and treated with aqueous 2N HCl (4 mL). The resulting mixture was stirred and heated at 60° C. for two hours, then cooled to room temperature and evaporated under vacuum to leave a yellow semi-solid. The residue was dissolved in EtOAc, washed with water and brine, dried over MgSO4, filtered, evaporated under vacuum, and stripped with toluene to afford 9a-butyl-4-(4-hydroxy-phenyl)-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (787 mg, ca. 92% weight pure) as a yellow foam.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07087599B2uspto-grants-2006_08