Hydrazine hydrate (1:1) → 4-(3-Chlorophenyl)pyridazine-3,6-diol
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:9](=O)[O:10][C:11](=[O:13])[CH:12]=2)[CH:5]=[CH:6][CH:7]=1.O.[NH2:16][NH2:17]>O.C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:12]=[C:11]([OH:13])[N:17]=[N:16][C:9]=2[OH:10])[CH:5]=[CH:6][CH:7]=1参加物
5
実験手順
To a 25 mL flask was added 3-(3-chlorophenyl)furan-2,5-dione (1.7 g, 8.15 mmol) from (1a) and hydrazine hydrate (0.476 mL, 9.78 mmol) in water (6 mL) and acetic acid (4 mL). The resulting mixture was refluxed for 18 hours. The solution was cooled and placed in the refrigerator for 1 hour. The resulting precipitate was filtered and dried, then purified by flash chromatography eluting with 5% methanol/dichloromethane to give 4-(3-chlorophenyl)pyridazine-3,6-diol.
後処理
- temperatureThe resulting mixture was refluxed for 18 hours
- temperatureThe solution was cooled
- filtrationThe resulting precipitate was filtered
- customdried
- custompurified by flash chromatography
- washeluting with 5% methanol/dichloromethane
出典と根拠
- ORDレコード
- ord-a2a103fb8fb34b94a6d33ca5cde93a59
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07723336B2
反応ノート
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