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Ammonia → 4,5-Dihydro-5-methyl-6-(4-(4-oxo-1(4H)-pyridinyl)phenyl)-3(2H)-pyridazinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4H-pyran-4-one | HCID 7968 | — |
| 反応物 | Ici 109,081 | HCID 161928 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,5-Dihydro-5-methyl-6-(4-(4-oxo-1(4H)-pyridinyl)phenyl)-3(2H)-pyridazinone | HCID 130702 | — |
反応手順
A stirred mixture of 6-(4-aminophenyl)-5-methyl-4,5-dihydro-3(2H)-pyridazinone (1.0 g), 4H-pyran-4-one (0.52 g), water (20 ml), and concentrated hydrochloric acid (0.41 ml) was heated under reflux for 31/2 hours. The resultant solid was dissolved in the minimum of hot water and the solution was neutralised with aqueous ammonia to give the crude product, 1.16 g, m.p. 249°-256° C. The product was recrystallised first from water to which a little 2N NaOH was added, and then from water alone to give the pure title compound, 0.82 g, m.p. 254°-256° C. (after melting and resolidifying at about 150° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246928 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-776b6e04372e48e3ab61b37e552959a1 |
| 出典メモ | uspto-grants-1993_09 |