Reaktion #48366

ord-393a1293af5f45da8e86eb6e83af40c9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe solution was cooled
  2. 2
    Sonstigepurged with argon, and 10% palladium on carbon
  3. 3
    workup.ADDITIONwas added (0.45 g)
  4. 4
    workup.ADDITIONHydrogen was introduced (1 atm)
  5. 5
    FiltrationThe catalyst was filtered
  6. 6
    Sonstigethe solvent evaporated from the filtrate

Vorschrift

2-Amino-6-methoxy-3-nitropyridine (2.8 g, 16.5 mmol) was dissolved in warm 1:1 methanol/ethanol (200 mL). The solution was cooled, purged with argon, and 10% palladium on carbon was added (0.45 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. MS 140 (M+1) 1H NMR (500 MHz, CDCl3) δ 6.93 (d, J=8 Hz, 1H), 6.04 (d, J=8 Hz, 1H), 4.15 (br s, 2H), 3.80 (s, 3H), 3.0 (br s, 2H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745427B2uspto-grants-2010_06