Sodium Hydroxide → 2,6-Diaminopyridine-3-carbonitrile
反応式
[NH2:1][C:2]1[N:10]=[C:9]([NH2:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=O.P(Cl)(Cl)(Cl)=O.[OH-].[Na+]>>[NH2:1][C:2]1[N:10]=[C:9]([NH2:11])[CH:8]=[CH:7][C:3]=1[C:4]#[N:6]参加物
4
反応条件
- 温度
- 100 °C
実験手順
2,6-Diamino-nicotinamide (520 mg) described in Manufacturing Example 7-1 and phosphorus oxychloride (5.0 g) were stirred for 0.5 hour at 100° C. The reaction solution was added to 0° C. dilute aqueous sodium hydroxide, which was then extracted with ethyl acetate. The organic layer was concentrated and the residue was purified with NH silica gel column chromatography (ethyl acetate) to obtain the titled compound (340 mg).
後処理
- extractionwas then extracted with ethyl acetate
- concentrationThe organic layer was concentrated
- customthe residue was purified with NH silica gel column chromatography (ethyl acetate)
出典と根拠
- ORDレコード
- ord-7f886482509f4db68bfcb5fd94c37ebe
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183264B2
反応ノート
読み込み中…