Hydrazine hydrate (1:1) → 5,8-Difluorophthalazine-1,4-dione
反応式
[F:1][C:2]1[CH:12]=[CH:11][C:10]([F:13])=[C:4]2[C:5]([O:7][C:8](=O)[C:3]=12)=[O:6].O.O.O.C([O-])(=O)C.[Na+].O.[NH2:23][NH2:24]>C(O)(=O)C>[F:1][C:2]1[CH:12]=[CH:11][C:10]([F:13])=[C:4]2[C:3]=1[C:8](=[O:7])[N:23]=[N:24][C:5]2=[O:6]参加物
5
実験手順
3,6-Difluorophthalic anhydride (10 g, 54 mmol) was added to a mixture of sodium acetate trihydrate (10 g, 73 mmol) and hydrazine hydrate (5 ml, 156 mmol) in 40% aqueous acetic acid. The reaction was heated under reflux conditions for 16 h and the reaction was filtered to give the title-compound as a white solid (10.5 g, 98%), 1H NMR (250 MHz, d6-DMSO) δ 8.01 (2H, t, J=9 Hz), 11.50-11.80 (2H, br s).
後処理
- temperatureThe reaction was heated under reflux conditions for 16 h
- filtrationthe reaction was filtered
出典と根拠
- ORDレコード
- ord-181bd68d594348d39b4b00977b3f2c50
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06200975B1
反応ノート
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