Water → 4-Bromopyridazine-3,6-diol
反応式
[Br:1][C:2]1[C:3](O[C:6](=[O:8])[CH:7]=1)=[O:4].C([O-])(=O)C.[Na+].O.[NH2:15][NH2:16].O>C(O)(=O)C.O>[Br:1][C:2]1[C:3](=[O:4])[NH:15][NH:16][C:6](=[O:8])[CH:7]=1参加物
6
反応条件
- 温度
- 100 °C
実験手順
A mixture of bromomaleic anhydride (50 g, 283 mmol) and sodium acetate (76.5 g, 562 mmol) in 40% acetic acid/water (750 ml) was treated with hydrazine monohydrate (16.5 ml, 339 mmol) at room temperature under nitrogen. The brown solution was stirred and heated at 100° C. for 18 hours. Upon cooling the mixture was poured into water (11) and extracted with ethyl acetate (6×500 ml). The combined extracts were dried (MgSO4), filtered and evaporated to afford the title compound (20 g, 37%) as an orange solid. 1H NMR (250 MHz, d6-DMSO) δ7.68 (1H, br s). MS (ES+) m/e 193 [MH]+, 191 [MH]+. This material was used without further purification.
後処理
- temperatureUpon cooling the mixture
- extractionextracted with ethyl acetate (6×500 ml)
- dry with materialThe combined extracts were dried (MgSO4)
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-8aca293d090446adaace60d29ff64fea
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06699859B1
反応ノート
読み込み中…