HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 5-Chloro-3,6-difluoropyridin-2-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 2-Amino-4-bromo-5-chloro-3,6-difluoropyridine | HCID 22121161 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 5-Chloro-3,6-difluoropyridin-2-amine | HCID 22121247 | 88.8% |
Reaction Steps
To 25 ml of methanol were added 2.7 g of 2-amino-4-bromo-5-chloro-3,6-difluoropyridine and 1.15 g of triethylamine together with 0.145 g of 10% palladium on carbon, and the mixture was hydrogenated at room temperature for 1.5 hours. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 50 ml of chloroform, and the mixture was washed with 30 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting colorless flake crystals were dispersed in a mixed solution of diisopropylether and n-hexane (1:2), and collected by filtration to obtain 1.62 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05998436 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-41d3b2fed4a0440baf800ee6836df483 |
| Source note | uspto-grants-1999_12 |