Реакция #2206839

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Растворители

Условия реакции

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

Обработка

  1. 1
    ТемператураAfter cooling to ca. 40° C.
  2. 2
    Экстракцияextracted with ethyl acetate (30 ml×3)
  3. 3
    ПромывкаThe combined organic layer was washed with brine (50 ml)
  4. 4
    Сушкаdried over magnesium sulfate
  5. 5
    Концентрированиеconcentrated in vacuo
  6. 6
    ПромывкаThe residue was washed with diisopropyl ether and ethyl acetate

Методика

To a solution warmed at 85° C. of (1,7-dimethyl-9-oxo-1,9-dihydro-4H-pyrazolo[4,3-b]quinolin-4-yl)acetonitrile (EXAMPLE 51, 69 mg, 0.27 mmol) in 2-methyl-2-propanol (5 ml) was added powdered potassium hydroxide (76 mg, 1.4 mmol). The mixture was stirred at 85° C. for 10 min. After cooling to ca. 40° C., the mixture was poured into water (30 ml) and extracted with ethyl acetate (30 ml×3). The combined organic layer was washed with brine (50 ml), dried over magnesium sulfate, and concentrated in vacuo. The residue was washed with diisopropyl ether and ethyl acetate to give 43 mg (59%) of the title compound as a yellow solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06686373B2uspto-grants-2004_02