HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azane;hydrate → (5-Fluoropyridin-3-yl)methanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azane;hydrate | HCID 12896473 | — |
| Reactant | (2,6-Dichloro-5-fluoropyridin-3-yl)methanamine | HCID 55255125 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | (5-Fluoropyridin-3-yl)methanamine | HCID 45116207 | — |
Reaction Steps
To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 28% NH3.H2O (50 ml) and a solution of (2,6-dichloro-5-fluoropyridin-3-yl)methanamine (Compound 144, 10.1 g, 52 mmol) in MeOH (100 ml). The mixture was placed under 51 psi H2 on a shaker type Parr apparatus for 16 h, filtered and concentrated. The resulting aqueous solution was basified with NaOH, extracted with EtOAc (×3). The combined organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The crude product was purified by distillation under vacuum to yield the title compound as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524917B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-47dd9896f15c4e0d94e5438076d71229 |
| Source note | uspto-grants-2013_09 |