Hydrazine hydrate (1:1) → 6,7-Dihydropyrido[2,3-d]pyridazine-5,8-dione
反応式
O.[NH2:2][NH2:3].[N:4]1[CH:9]=[CH:8][CH:7]=[C:6]2[C:10](O[C:13](=[O:14])[C:5]=12)=[O:11].C([O-])(=O)C.[Na+]>C(O)(=O)C.O>[N:4]1[C:5]2[C:13](=[O:14])[NH:2][NH:3][C:10](=[O:11])[C:6]=2[CH:7]=[CH:8][CH:9]=1参加物
5
実験手順
Hydrazine hydrate (13.09 g, 0.261 mol) was added to a stirred solution of pyridine-2,3-dicarboxylic anhydride (30.0 g, 0.201 mol) and sodium acetate (21.45 g, 0.261 mol) in 40% acetic acid/water (400 ml). The reaction was heated at reflux for 3 days under nitrogen. The yellow precipitate was filtered off and washed successively with water (4×200 ml), hexane (3×150 ml) and diethyl ether (3×150 ml) to give the title-compound (25.0 g, 76%), 1H NMR (250 MHz, d6-DMSO) δ 7.90 (1H, q, J=4.5Hz, Ar—H), 8.51 (1H, d, J=4.5Hz, Ar—H), 9.13 (1H, d, J=4.6Hz, Ar—H), 11.65 (2H, br s, 2 of NH); MS (ES+) m/e 164 [MH]+.