反应 #48373

ord-f06cba3385d146d3b17067dc2a249813

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the mixture was filtered
  2. 2
    洗涤rinsed with more tetrahydrofuran
  3. 3
    浓缩concentrated
  4. 4
    workup.DISSOLUTIONThis residue was dissolved in ethanol (50 mL)
  5. 5
    其他purged 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
    过滤The catalyst was filtered
  9. 9
    其他the solvent evaporated from the filtrate

实验过程

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)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07745427B2uspto-grants-2010_06