Hydrazine hydrate (1:1) → 5-Bromo-2-hydrazinopyridine

To a solution of 5-bromo-2-fluoropyridine (10 g, 56.8 mmol) in EtOH (120 ml) was added hydrazine hydrate (14.22 g, 284 mmol), the mixture was heated to reflux and stirred overnight (16 hr). The solvent of the reaction mixture was evaporated about half under reduced pressure, then cooling in an ice bath there precipitation was occurred, filtered and washed the product with a minimum of EtOH and water, dried in vacuum to obtain pure desired product as white powder (10.2 g, yield 91%). LCMS (method A): [M+H]+=188.1, 190.1, tR=0.62 min.

1. temperaturethe mixture was heated
2. temperatureto reflux
3. customThe solvent of the reaction mixture was evaporated about half under reduced pressure
4. temperaturecooling in an ice bath
5. customthere precipitation
6. filtrationfiltered
7. washwashed the product with a minimum of EtOH and water
8. customdried in vacuum

ORD record

ord-3e984cee95864ee2a2a5127ab59dbe2b

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09062045B2