Реакция #600394

ord-32b09f46a1bf42d2b54a87d4ee296622

Растворители

Условия реакции

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

Обработка

  1. 1
    Температураcooled to r.t
  2. 2
    ФильтрацияThe resulting solids were filtered
  3. 3
    Другоеazeotroped with EtOAc (2 L)
  4. 4
    Другоеdried overnight at 40° C. under vacuum and nitrogen sweep

Методика

To a solution of 3-chloropyrazin-2-amine (52 g, 401 mmol) in acetonitrile (750 mL) under N2 was added sodium bicarbonate (67.4 g, 803 mmol), and then methyl bromopyruvate (97 mL, 803 mmol). The mixture was then heated to 80° C. for 4 hours and then cooled to r.t. The reaction was then diluted water (2200 mL) and stirred for 30 minutes. The resulting solids were filtered, azeotroped with EtOAc (2 L), and dried overnight at 40° C. under vacuum and nitrogen sweep to give the title compound (60 g). LRMS (ESI) calc (M+H)+=212.0. found 212.0

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09102673B2uspto-grants-2015_08