تفاعل #48373

ord-f06cba3385d146d3b17067dc2a249813

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe mixture was filtered
  2. 2
    غسيلrinsed with more tetrahydrofuran
  3. 3
    تركيزconcentrated
  4. 4
    workup.DISSOLUTIONThis residue was dissolved in ethanol (50 mL)
  5. 5
    أخرىpurged 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
    ترشيحThe catalyst was filtered
  9. 9
    أخرىthe solvent evaporated from the filtrate

الإجراء التجريبي

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)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745427B2uspto-grants-2010_06