反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=O)[CH:2]=1.[NH2:9][NH2:10]>CO>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][NH:9][NH2:10])[CH:2]=1参加物
4
実験手順
To a solution of pyridine-3-aldehyde (5 g, 46.7 mmol) in methanol (100 mL) was added hydrazine (1.05 mL, 46.7 mmol). The reaction mixture was stirred at rt for 1 h. After purging with nitrogen, 10% Pd/C (200 mg) was added. The reaction mixture was purged with hydrogen and stirred under hydrogen at rt overnight. Solid material was removed, and the filtrate was concentrated to give a crude Example 85A. This material was used without further purification. Yield: 5.2 g (91%). MS (DCI): m/z 124 (M+H)+.
後処理
- customAfter purging with nitrogen, 10% Pd/C (200 mg)
- additionwas added
- customThe reaction mixture was purged with hydrogen
- stirringstirred under hydrogen at rt overnight
- customSolid material was removed
- concentrationthe filtrate was concentrated
- customto give a crude Example 85A
- customThis material was used without further purification
出典と根拠
- ORDレコード
- ord-2da334fd40f241b9bbdcd2169755c65e
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08546368B2
関連ノート
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