Реакция #88076

ord-37341f31c3054b56b8b8bd7b6fad65fe

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеAfter removal of methanol, water (20 mL)
  2. 2
    workup.ADDITIONwas added to the residue
  3. 3
    workup.ADDITIONthe resulting solution was basified by addition of sodium hydroxide to pH=13
  4. 4
    ЭкстракцияThe aqueous solution was extracted with dicholromethane
  5. 5
    Сушкаthe combined organic phase was dried over sodium sulfate
  6. 6
    ДругоеRemoval of the solvent under reduced pressure

Методика

To a solution of 1-pyrazin-2-yl-ethanone (2.0 g, 15.85 mmol) and ammonium acetate (19.337 g, 158.5 mmol) in methanol (50 mL) was added sodium cyanoborohydride (0.7 g, 11.1 mmol) in one portion. The reaction mixture was stirred overnight at room temperature. After removal of methanol, water (20 mL) was added to the residue and the resulting solution was basified by addition of sodium hydroxide to pH=13. The aqueous solution was extracted with dicholromethane and the combined organic phase was dried over sodium sulfate. Removal of the solvent under reduced pressure afforded 14.62 g of 1-pyrazin-2-yl-ethylamine, yield: 75%. MS (M+H)=124.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09440956B2uspto-grants-2016_09