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

Temperature

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 record

ord-98111954b62943be9c1eb4e0e8c5d304

Source dataset

uspto-grants-2002_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06348474B1