Phosphorus oxychloride → 3-Amino-5-morpholinopicolinonitrile
反応式
[NH2:1][C:2]1[C:3]([C:14]([NH2:16])=O)=[N:4][CH:5]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:7]=1.P(Cl)(Cl)(Cl)=O>C(#N)C>[NH2:1][C:2]1[C:3]([C:14]#[N:16])=[N:4][CH:5]=[C:6]([N:8]2[CH2:9][CH2:10][O:11][CH2:12][CH2:13]2)[CH:7]=1参加物
4
実験手順
A stirred solution of 3-amino-5-morpholinopicolinamide (0.35 g, 1.57 mmol) in acetonitrile (10 mL) was treated with phosphorus oxychloride (0.29 mL, 3.15 mmol). The reaction was heated at reflux for 1 h. After this time the reaction was cooled to rt and evaporated in vacuo. The residue was dissolved in Et2O (10 mL) and treated with 4.0M HCl in dioxane (0.2 mL). The resulting solid was filtered and dried under vacuum to give 3-amino-5-morpholinopicolinonitrile. Mass Spectrum (ESI) m/e=205.2 (M+1).
後処理
- temperatureThe reaction was heated
- temperatureat reflux for 1 h
- customevaporated in vacuo
- dissolutionThe residue was dissolved in Et2O (10 mL)
- additiontreated with 4.0M HCl in dioxane (0.2 mL)
- filtrationThe resulting solid was filtered
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-f3d7308b25604fb2848e703a88694e44
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08940724B2
反応ノート
読み込み中…