HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86629437, compound → HCID 67062977, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86629437 | HCID 86629437 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67062977 | HCID 67062977 | 66.4% |
Reaction Steps
A solution 3-(4-fluoro-3-nitrophenyl)-7-(methoxy(methyl)amino)-1-methyl-3,4-dihydropyrido[4,3-d]pyrimidin-2(1H)-one (2 g, 5.5 mmol) in methanol (30 mL) was stirred with 10% Pd/C (1.0 g, 0.94 mmol) under hydrogen (45 psi) at 45° C. for 24 h. The complete reaction mixture was filtered, and the filtrate was concentrated in vacuo. The residue was washed with ethyl ether and dried in vacuo to provide 3-(3-amino-4-fluorophenyl)-1-methyl-7-(methylamino)-3,4-dihydropyrido[4,3-d]pyrimidin-2(1H)-one (1.1 g, 66% yield). 1H NMR (400 MHz, DMSO-d6): δ 7.70 (s, 1 H), 6.94 (t, J=9.6 Hz, 1 H), 6.66 (d, J=6.8 Hz, 1 H), 6.40 (m, 2H), 5.92 (s, 1 H), 5.17 (s, 2 H), 4.50 (s, 2 H), 3.13 (s, 3 H), 2.73 (d, J=4.0 Hz, 3 H), MS (ESI) m/z: 302.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897762B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-ab1d2aac69834d16a83552f274d27bb2 |
| Source note | uspto-grants-2011_03 |