HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-carboxy-6-(3-fluoro-4-methylphenyl)-2H-pyridazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | Ethyl 2-ethoxycarbonyl-4-(3-fluoro-4-methylphenyl)-2-hydroxy-4-oxobutanoate | HCID 21991669 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 4-carboxy-6-(3-fluoro-4-methylphenyl)-2H-pyridazin-3-one | HCID 21991555 | — |
Reaction Steps
To a solution of ethyl 2-ethoxycarbonyl-4-(3-fluoro-4-methylphenyl)-2-hydroxy-4-oxobutanoate (8.41 9, 25.8 mmol) in isopropanol (100 mL) was added hydrazine monohydrate (2.84 g, 56.8 mmol), and the mixture was heated under stirring at 100 for 6 hours. Then, 2 mol/L sodium hydroxide was added, and the mixture was stirred further at the same temperature for 4 hours. The reaction mixture was ice-cooled, and concentrated hydrochloric acid was added to acidify the system. The precipitate was collected by filtration, thoroughly washed with water and dried to yield the title compound as a slightly yellow crystalline powder (5.67 g, 87.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07087606B2 |
| Source dataset | uspto-grants-2006_08 |
| ORD ID | ord-e9eae8e4020a414d90a4fd0e994de72c |
| Source note | uspto-grants-2006_08 |