Реакция #53613

ord-5b002fe2b46341b88a3c9b37213119a9

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Концентрированиеconcentrated under reduced pressure
  2. 2
    workup.ADDITIONIce-water was added to the residue, which
  3. 3
    Экстракцияextracted with ethyl acetate
  4. 4
    ПромывкаThe extracts were washed with brine
  5. 5
    Сушкаdried over anhydrous magnesium sulfate
  6. 6
    Концентрированиеconcentrated under reduced pressure
  7. 7
    ДругоеThe residue obtained
  8. 8
    Другоеwas chromatographed on silica gel in ethyl acetate:hexane (1:2)

Методика

Trifluoroacetic acid 1 ml and water 0.1 ml were added to compound (34) 48.4 mg. The mixture was heated at 80° C. for 15 min and concentrated under reduced pressure. Ice-water was added to the residue, which was made alkaline with an aqueous saturated sodium hydrogen carbonate solution and extracted with ethyl acetate. The extracts were washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was chromatographed on silica gel in ethyl acetate:hexane (1:2) to give the titled compound (35) as a colorless oil, 33.2 mg. Yield 78%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06858640B2uspto-grants-2005_02