Реакция #71322

ord-38ce25d16e14442dade8dbee01847460

Растворители

Условия реакции

Температура
150°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеwas obtained),
  2. 2
    Температураto cool to rt
  3. 3
    Экстракцияextracted with Et2O
  4. 4
    workup.ADDITIONThe aqueous phase was acidified to pH 5 by addition of HCl
  5. 5
    ФильтрацияVacuum filtration of the resulting suspension

Методика

KOH (6.0 g, 107 mmol, 10 equiv) was added to 8-(3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile (Step 1.3) (3.12 g, 10.7 mmol) in ethylene glycol (30 mL). The reaction mixture was stirred at 150° C. for 3 h (a solution was obtained), allowed to cool to rt, diluted with Et2O/H2O, and extracted with Et2O. The aqueous phase was acidified to pH 5 by addition of HCl. Vacuum filtration of the resulting suspension afforded 3.3 g of the title compound as a yellow solid: ESI-MS: 311.0 [M+H]+; tR=4.34 min (System 1).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08536175B2uspto-grants-2013_09