HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 2-(t-Butylamino)-5-chloro-3,6-difluoropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 4-Bromo-2-(t-butylamino)-5-chloro-3,6-difluoropyridine | HCID 22121170 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 2-(t-Butylamino)-5-chloro-3,6-difluoropyridine | HCID 22121189 | 98.6% |
Reaction Steps
To 30 ml of methanol were added 12.8 g of 4-bromo-2-(t-butylamino)-5-chloro-3,6-difluoropyridine and 2.5 g of triethylamine together with 0.57 g of 10% palladium on carbon, and the mixture was hydrogenated at 50° C. for 5 days. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 80 ml of chloroform, and the mixture was washed with 70 ml of distilled water, and the chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 9.3 g of the title compound as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05998436 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-667ff37515af48358fc5cd7d0b018db3 |
| Source note | uspto-grants-1999_12 |