Pyridine-2-carbonitrile → Cqp4A25CE2
反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)#[N:2].O.[NH2:10][NH2:11]>CCO>[CH:7]1[CH:8]=[C:3](/[C:1](/[NH2:2])=[N:10]\[NH2:11])[N:4]=[CH:5][CH:6]=1参加物
4
反応条件
- 温度
- 0 °C
実験手順
2-Cyano pyridine (500 mg, 1.923 mmol) and Hydrazine hydrate (252 mg, 1.923 mmol) were mixed together in EtOH (3 ml). The clear solution was left at 15° C. (in refrigerator) for 18 h (Monitored by TLC). Ethanol was concentrated under reduced pressure and then the reaction mixture was diluted with diethyl ether (50 ml) and water. The diethyl ether layer was separated, washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to 1/5th Volume. The ethereal solution was cooled to 0° C. and the obtained solid precipitate was collected over the filtration and dried under vacuum, which gave the 2-pyridine Amidrazone (360 mg).
後処理
- concentrationEthanol was concentrated under reduced pressure
- additionthe reaction mixture was diluted with diethyl ether (50 ml) and water
- customThe diethyl ether layer was separated
- washwashed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure to 1/5th Volume
- filtrationthe obtained solid precipitate was collected over the filtration
- customdried under vacuum, which
出典と根拠
- ORDレコード
- ord-69fecea4563a43a794e7340f3caa5c4e
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07829589B2
反応ノート
読み込み中…