Ethanol → 2-Amino-6-bromo-3-methoxypyridine

Temperatur

72.5 °C

To a heterogeneous solution of 6-bromo-3-methoxy-2-nitropyridine (32) (2.32 g, 10 mmol) in of ethanol:water (40 mL, each) were added iron powder (2.8 g, 50 mmol), followed by ammonium chloride (2.64 g, 50 mmol) at room temperature. The resulting heterogeneous mixture was then stirred at 70-75° C. for 15 minutes, filtered through celite (when hot), washed with ethanol (2×50 mL) and solvent was then removed under reduced pressure. The residue upon dilution with water afforded a solid, which was isolated by filtration to give 2-amino-6-bromo-3-methoxypyridine (33). LCMS: purity: 95%, MS (m/z): 203 (MH+).

1. filtrationfiltered through celite (when hot)
2. washwashed with ethanol (2×50 mL) and solvent
3. customwas then removed under reduced pressure
4. customThe residue upon dilution with water afforded a solid
5. customwhich was isolated by filtration

ORD-Eintrag

ord-340ff2ab30cd417f800fa3fc0966e626

Quelldatensatz

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08399472B2