HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylhydrazine → 6-methyl-2-{[4-(4-methylpiperazin-1-yl)phenyl]amino}-8-phenylpyrimido[4,5-d]pyridazin-5(6H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | HCID 71224273 | HCID 71224273 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | 6-methyl-2-{[4-(4-methylpiperazin-1-yl)phenyl]amino}-8-phenylpyrimido[4,5-d]pyridazin-5(6H)-one | HCID 71224006 | — |
Reaction Steps
A solution of Example 3B (50 mg, 0.112 mmol) and methylhydrazine (6.50 μl, 0.123 mmol) in n-butanol (12.5 mL) was heated to 170° C. by microwave irradiation (Biotage Initiator) for 3 hour. The reaction mixture was cooled to room temperature, and the solid was filtered and air-dried to provide the title compound. MS ESI(+) m/z 428.2 [M+H]+; 1H NMR (300 MHz, DMSO-d6): δ ppm 10.34 (s, 1H), 9.29 (s, 1H), 7.94-7.91 (m, 2H), 7.59-7.48 (m, 5H), 6.84 (d, J=8.7 Hz, 2H), 3.75 (s, 3H), 3.13-3.05 (m, 4H), 2.47-2.44 (m, 4H), 2.22 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796289B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-1a47ad3b13ff41b4a1cf9781ecd63ca3 |
| Source note | uspto-grants-2014_08 |