HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 19012219, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 4,6-Dimethyl-3,5-dinitropyridin-2-amine | HCID 19754069 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladiumcarbon | HCID 14818447 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19012219 | HCID 19012219 | — |
Reaction Steps
A 500 ml Parr Bottle was charged with 2-amino-4,6-dimethyl-3,5-dinitropyridine (21.2 g, 0.10 mole), 200 ml methanol, methanesulfonic acid (19.2 g, 0.20 mole), and 20.g 5% Pd/charcoal catalyst. The mixture was subjected to hydrogenation at ambient temperature with an initial hydrogen pressure of 5.7 psig. When no further uptake of hydrogen was observed, the mixture was filtered free of catalyst under a nitrogen atmosphere, and methanol removed under vacuum. The bismethanesulfonate salt of 2,3,5-triamino-4,6-dimethylpyridine so obtained was purified by slurrying with dry isopropyl alcohol, filtering under nitrogen, and vacuum drying over P2O5 at 80°-90° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04022793 |
| Source dataset | uspto-grants-1977_05 |
| ORD ID | ord-1506e3d2b65044adb80101c8b37ece72 |
| Source note | uspto-grants-1977_05 |