Реакция #8089

ord-91f9a9d242cc4d829d962d9a6373321d

Растворители

Условия реакции

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

Обработка

  1. 1
    Другоеto drop back to room temperature
  2. 2
    ЭкстракцияThe mixture was then extracted with ethyl acetate
  3. 3
    ПромывкаThe extract was washed with brine
  4. 4
    Сушкаdried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    Другоеthe residue was reacted

Методика

To a solution of 4-methoxycarbonyl-6-[4-(methylthio)-phenyl]-2H-pyridazin-3-one (8.00 g, 29.0 mmol) in N,N-dimethylformamide (80 mL) were added potassium carbonate (8.02 g, 58.0 mmol) and isobutyl bromide (4.76 g, 34.8 mmol), and the mixture was stirred at 80° C. for 2 hours. The temperature of the reaction mixture was allowed to drop back to room temperature, and a saturated aqueous solution of sodium hydrogencarbonate was added. The mixture was then extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was distilled off. Following the procedure of Example 1 (7), the residue was reacted to yield the title compound as a yellow solid [yield: 65.1% (2 steps)].

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07087606B2uspto-grants-2006_08