Hydrazine hydrate (1:1) → 4-(3-Chlorophenyl)pyridazine-3,6-diol

HRID 2239888ノート

反応式

HRID 2239888 の反応式
[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

  1. temperatureThe resulting mixture was refluxed for 18 hours
  2. temperatureThe solution was cooled
  3. filtrationThe resulting precipitate was filtered
  4. customdried
  5. custompurified by flash chromatography
  6. 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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