Реакция #47827

ord-dcc48670644f41dbafba0d9dcc7475a0

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураrefluxed for 1 hr
  2. 2
    ПромывкаThe resulting mixture washed with saturated sodium bicarbonate
  3. 3
    Экстракцияextracted with ethyl acetate
  4. 4
    ДругоеThe organic layer was separated
  5. 5
    Сушкаdried over anhydrous MgSO4
  6. 6
    Концентрированиеconcentrated under a reduced pressure
  7. 7
    ДругоеThe resulting residue was purified by flash chromatography

Методика

6-Methoxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (1.6 g, 5.19 mmol) obtained in Example 1 was dissolved in ethanol (100 mL), hydroxylamine hydrochloride (1.08 g, 15.57 mmol) and pyridine (1.64 g, 1.68 mL, 20.76 mmol) were added thereto, refluxed for 1 hr, and cooled to RT. The resulting mixture washed with saturated sodium bicarbonate and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 1.34 g of the titled compound (yield: 80%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07745439B2uspto-grants-2010_06