Реакция #7957

ord-58e5100c1cca454d952bc1df3a46b49a

Растворители

Условия реакции

Температура
85°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураOn cooling
  2. 2
    ТемператураThe mixture was cooled in an ice bath
  3. 3
    Фильтрацияfiltered
  4. 4
    ПромывкаThe crystalline product was washed with ice-cold 5:1 MeOH-2N HCl (2×2 mL)
  5. 5
    Другоеdried under vacuum

Методика

A solution of (2SR,9aRS)-9a-butyl-2,4-dimethyl-7-methoxymethoxy-2-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (40 mg, 0.11 mmol) in methanol (approx. 0.5-1 mL) was placed under a nitrogen atmosphere and treated with 2N aqueous HCl (0.165 mL, 0.37 mmol). The resulting yellow solution was stirred and heated in an oil bath at 85° C. for 60 minutes. On cooling, the mixture deposited white crystals. The mixture was cooled in an ice bath and filtered. The crystalline product was washed with ice-cold 5:1 MeOH-2N HCl (2×2 mL) and dried under vacuum to afford (2SR,9aRS)-9a-butyl-2,4-dimethyl-7-hydroxy-2-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.

Источник

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