Water → HCID 178516183, compound

5-Bromo-4-chloropyridin-2-amine (2.01 g, 9.69 mmol) was dissolved in 75% (v/v) sulfuric acid (40.2 mL, 566 mmol) and then chilled in an ice bath. A solution of sodium nitrite (2.21 g, 32.0 mmol) in water (20.1 mL, 1116 mmol) was added drop-wise and the reaction mixture was then stirred for 3 hours. The mixture was concentrated under reduced pressure and aqueous ammonia (15 mL) was added drop-wise. The resulting white precipitate was collected via vacuum filtration and the filter cake washed with cold water (100 mL) then dried in a vacuum oven for 24 hours to give 1.94 g (95%) of the title compound.

1. temperaturechilled in an ice bath
2. concentrationThe mixture was concentrated under reduced pressure and aqueous ammonia (15 mL)
3. additionwas added drop-wise
4. filtrationThe resulting white precipitate was collected via vacuum filtration
5. washthe filter cake washed with cold water (100 mL)
6. customthen dried in a vacuum oven for 24 hours

ORD record

ord-fa28a2ad96634502aefc3398c45c5520

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09428514B2