HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenylhydrazine → 1-(3-methoxyphenyl)-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4(1H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenylhydrazine | HCID 7516 | — |
| Reactant | 3-[3-(dimethylamino)prop-2-enoyl]-1-(3-methoxyphenyl)pyridazin-4(1H)-one | HCID 66710990 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-(3-methoxyphenyl)-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4(1H)-one | HCID 46219453 | 14% |
Reaction Steps
To a solution of 3-[3-(dimethylamino)prop-2-enoyl]-1-(3-methoxyphenyl)pyridazin-4(1H)-one (crude 640 mg, 2.14 mmol) in 20 mL of methanol was added phenylhydrazine (347 mg, 3.21 mmol). The mixture was refluxed for 4 h and concentrated. The residue was dissolved in dichloromethane (20 mL), washed with 1N HCl aqueous solution and brine, dried over Na2SO4, and concentrated under reduced pressure. The residue was purified by prep-HPLC to give 1-(3-methoxyphenyl)-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4(1H)-one (106 mg, 14% for two steps) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513251B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-88783191ac5643278b454ff0a487005e |
| Source note | uspto-grants-2013_08 |