Hydrogen Bromide → 6-Bromo-3-nitro-2-pyridinamine

Temperatur

100 °C

A 30% solution of hydrogen bromide in acetic acid (10 ml) was added to 2-amino-6-chloro-3-nitropyridine (1.0 g) at room temperature and the mixture was heated at 100° C. After 24 hr, a 30% solution of hydrogen bromide in acetic acid (5 ml) was added. After 48 hr, the reaction mixture was cooled and concentrated. The residue was neutralized with 28% aqueous ammonia and extracted three times with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was crystallized from isopropyl ether to give the objective compound (1.14 g) as yellow crystals.

1. waitAfter 48 hr
2. temperaturethe reaction mixture was cooled
3. concentrationconcentrated
4. extractionextracted three times with ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was crystallized from isopropyl ether

ORD-Eintrag

ord-4bd694c7b0a84d14bc5a8ab1317d6890

Quelldatensatz

uspto-grants-2005_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06911469B2