Hydrochloric Acid → HCID 59394182、化合物
反応式
[CH3:1][C:2]1([C:5](=O)[CH2:6][C:7]#[N:8])[CH2:4][CH2:3]1.Cl.[CH3:11][NH:12][NH2:13]>CCO.O1CCOCC1>[CH3:11][N:12]1[C:5]([C:2]2([CH3:1])[CH2:4][CH2:3]2)=[CH:6][C:7]([NH2:8])=[N:13]1参加物
6
実験手順
To a solution of 3-(1-methyl-cyclopropyl)-3-oxo-propionitrile (1.0 g, 8.1 mmol) in EtOH (10 mL) is added 4N HCl in Dioxane (10 mL). The mixture is stirred at room temperature for 16 hour. Concentrated under reduced pressure, the residue is dissolved in MeOH (40 mL) and treated with methylhydrazine (0.56 g, 12.2 mmol). The mixture is heated at 80° C. for 16 h. The solution is then concentrated in vacuo and the residue is purified by HPLC give product. MS (ESI) m/z 152.3 (M+1).
後処理
- concentrationConcentrated under reduced pressure
- dissolutionthe residue is dissolved in MeOH (40 mL)
- temperatureThe mixture is heated at 80° C. for 16 h
- concentrationThe solution is then concentrated in vacuo
- customthe residue is purified by HPLC
- customgive product
出典と根拠
- ORDレコード
- ord-c7596535551b46808afd473288048023
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541432B2
反応ノート
読み込み中…