Реакция #1751928

ord-78cf78201db548c997442d63a551b327

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Фильтрацияthe mixture was filtered
  2. 2
    Промывкаrinsed with more tetrahydrofuran
  3. 3
    Концентрированиеconcentrated
  4. 4
    workup.DISSOLUTIONThis residue was dissolved in ethanol (50 mL)
  5. 5
    Другоеpurged with argon, and 10% palladium on carbon
  6. 6
    workup.ADDITIONwas added (0.15 g)
  7. 7
    workup.ADDITIONHydrogen was introduced (1 atm)
  8. 8
    ФильтрацияThe catalyst was filtered
  9. 9
    Другоеthe solvent evaporated from the filtrate

Методика

The HCl salt of 3-azido-5-fluoropyridin-2-amine (1.90 g, 10.0 mmol) was dissolved in tetrahydrofuran (100 mL) and treated with MP-Carbonate (Argonaut, 11.5 g). After 1 h, the mixture was filtered, rinsed with more tetrahydrofuran, and concentrated. This residue was dissolved in ethanol (50 mL), purged with argon, and 10% palladium on carbon was added (0.15 g). Hydrogen was introduced (1 atm) and the reaction stirred until complete. The catalyst was filtered and the solvent evaporated from the filtrate to give the title compound (1.18 g). MS 128.0 (M+1)

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08039460B2uspto-grants-2011_10