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Hydrazine hydrate (1:1) → 6-(4-Bromophenyl)-4,5-dihydropyridazin-3(2H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 3-(4-Bromobenzoyl)propionic acid | HCID 80646 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-(4-Bromophenyl)-4,5-dihydropyridazin-3(2H)-one | HCID 689108 | 98.3% |
反応手順
4-(4-Bromo-phenyl)-4-oxo-butyric acid (Aldrich, 25.0 g, 97.3 mmol) was treated with NH2NH2—H2O (Aldrich, 55%, 9.1 mL, 156 mmol) in EtOH (Aldrich, 100 mL) at refluxing for 2 h. It was cooled down to ambient temperature and the white solid was filtered off to give the title compound (24.2 g, 98%). 1H NMR (CDCl3, 300 MHz) δ 2.50-2.76 (m, 2H), 2.85-3.09 (m, 2H), 7.43-7.71 (m, 4H), 8.55 (s, 1H) ppm. MS (DCl/NH3) m/z 253 (M+H)+, 255 (M+H)+, 270 (M+NH4)+, 272 (M+NH4)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07309699B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-f40bd48d7f084095af3e1c39053a635a |
| 出典メモ | uspto-grants-2007_12 |