HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → 5-Bromo-3-fluoro-2-hydrazinylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 5-Bromo-2,3-difluoropyridine | HCID 14549654 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 5-Bromo-3-fluoro-2-hydrazinylpyridine | HCID 53402980 | 94.6% |
Reaction Steps
To a solution of 5-bromo-2,3-difluoropyridine (15 g, 77 mmol)) in EtOH (250 ml) was added hydrazine hydrate (19.36 g, 387 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 (15 g, yield 94%). LCMS (method A): [M+H]+=206.0, 208.0, tR=1.01 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062045B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-15fd6bafa7bb42848e26d1c8772d79c4 |
| Source note | uspto-grants-2015_06 |