HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68985826, compound → HCID 69297923, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68985826 | HCID 68985826 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 69297923 | HCID 69297923 | 47% |
Reaction Steps
A solution of Example A3 (2.5 g, 7.9 mmol) in EtOH (30 ml) was treated with Raney Nickel® (50% slurry in water, 10 g, 85 mmol) and the mixture was refluxed for 3 h. The cooled reaction was filtered and the filtrate was concentrated to give the crude product, which was washed with cold MeOH (2 mL) to give 6-(3-amino-4-fluoro-phenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one (1.0 g, 47% yield). 1H NMR (300 MHz, DMSO-d6)δ 9.10 (s, H), 9.07 (s, 1 H), 8.06 (s, 1 H), 7.14 (dd, J=8.7, 2.1 Hz, 1 H), 7.05 (dd, J=11.4, 8.4 Hz, 1 H), 6.82 (m, 1 H), 5.22 (s, 2 H), 3.68 (s, 3 H); MS (ESI) m/z: 271.3 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188113B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-bb406dcd2a1b42c7a7d711226667a548 |
| Source note | uspto-grants-2012_05 |