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Potassium Carbonate → 4-Chloro-5-methoxy-2-phenyl-3(2H)-pyridazinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4,5-Dichloro-2-phenyl-3(2H)-pyridazinone | HCID 72813 | — |
| 反応物 | HCID 18991304 | HCID 18991304 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Chloro-5-methoxy-2-phenyl-3(2H)-pyridazinone | HCID 349842 | 95% |
反応手順
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)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07001895B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-71bb804fd7f74371a69d8cbe36c7d532 |
| 出典メモ | uspto-grants-2006_02 |