Methylamine → 5-Chloro-4-methylamino-nicotinonitrile
反応式
Cl[C:2]1[C:7]([C:8]#[N:9])=[CH:6][N:5]=[CH:4][C:3]=1[Cl:10].[CH3:11][NH2:12]>>[Cl:10][C:3]1[CH:4]=[N:5][CH:6]=[C:7]([C:2]=1[NH:12][CH3:11])[C:8]#[N:9]参加物
3
反応条件
- 温度
- 60 °C
実験手順
4,5-Dichloronicotinonitrile (500 mg, 2.89 mmol) was suspended in 41% aqueous methylamine solution (5 mL). The resultant mixture was heated, with stirring, up to 60° C. over ca. 30 min. The mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer was washed with water, followed by brine then dried (MgSO4) and evaporated to provide the title compound (340 mg, 70%) as a white solid. 1H NMR (CDCl3) 8.39 (1H, s), 8.29 (1H, s), 5.50 (1H, s, br), 3.43 (3H, d, J=5.5 Hz).
後処理
- temperatureThe mixture was cooled to room temperature
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialthen dried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-d90611d3a6124014bb45ab3784c4e4c1
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07855216B2
反応ノート
読み込み中…