HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → 4-Chloro-5-methoxy-2-phenyl-3(2H)-pyridazinone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4,5-Dichloro-2-phenyl-3(2H)-pyridazinone | HCID 72813 | — |
| Edukt | HCID 18991304 | HCID 18991304 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 4-Chloro-5-methoxy-2-phenyl-3(2H)-pyridazinone | HCID 349842 | 95% |
Reaktionsschritte
The title compound was prepared according to the method of (S. Cho et al. described in J. Het. Chem., (1996), 33, 1579-1582), starting with the N-phenyl-dichloropyridazinone. A mixture of 2-phenyl-4,5-dichloro-3(2H)-pyridazinone (1 g, 4.1 mmol) and finely powdered, anhydrous K2CO3 (580 mg, 4.2 mmol) in 50 mL of methanol was heated at reflux for 5 hours and concentrated in vacuo. The residue was partitioned between water and ethyl acetate. The acetate layer was washed with water, and brine to provide 2-phenyl-4-chloro-5-methoxy-3(2H)-pyridazinone (yield: 920 mg, 95%). 1H NMR (300 MHz, DMSO-d6) δ 4.15 (s, 3H), 7.50 (m, 5H), 8.43 (s, 1H). MS (DCI/NH3) m/z 237 (M+H)+, 254 (M+NH4)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06307047B1 |
| Quelldatensatz | uspto-grants-2001_10 |
| ORD ID | ord-926ab51aac9f4bd69fa2bfa9d76580d3 |
| Quellennotiz | uspto-grants-2001_10 |