HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 70663178, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 6-chloro-4-(5-fluoro-2-methylphenyl)-N-methylpyridin-3-amine | HCID 57710450 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 70663178 | HCID 70663178 | — |
Reaction Steps
A solution of 6-chloro-4-(5-fluoro-2-methylphenyl)-N-methylpyridin-3-amine (0.2 g, 798 μmol, example 253, intermediate a) in EtOAc (1 mL) and MeOH (1.0 mL) under argon was treated with palladium on carbon (21.2 mg, 19.9 μmol) and stirred under an hydrogen atmosphere (0.5 bar overpressure) for 4 hours. Stirring was continued overnight at room temperature. The reaction mixture was filtered over Dicalite and evaporated. The residue was taken up in CH2Cl2 and saturated aqueous NaHCO3 solution and the layers were separated. The aqueous layer was extracted three times with CH2Cl2. The organic layers were dried over MgSO4, filtered and evaporated. Light brown solid (0.16 g; 92%). MS (ESI): m/z=217.11 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08987307B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-f0cd62b0fc354843af2f97972a2ae5d7 |
| Source note | uspto-grants-2015_03 |