Dimethylformamide dimethyl acetal → HCID 178526359、化合物
反応式
[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH2:9])[CH:4]=1.C[N:11]([CH:13](OC)OC)C.N[OH:19].Cl>CC(O)C>[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH:9][CH:13]=[N:11][OH:19])[CH:4]=1参加物
5
反応条件
- 温度
- 90 °C
実験手順
To a solution of 4-(chloromethyl)pyridin-2-amine (4-1) (1.56 g, 8.7 mmol) in propan-2-ol (15 mL) was added DMF-DMA (1.56 mL, 11.3 mmol) at room temperature under N2. The reaction mixture was heated to 90° C. for 3 h. After cooled to 50° C., the mixture was treated with NH2OH.HCl (0.781 g, 11.3 mmol), then stirred at 50° C. overnight. After cooled to room temperature, the mixture was concentrated and purified by chromatography on silica gel to afford the title compound (820 mg). MS (m/z): 186 (M+1)+.
後処理
- temperatureAfter cooled to 50° C.
- temperatureAfter cooled to room temperature
- concentrationthe mixture was concentrated
- custompurified by chromatography on silica gel
出典と根拠
- ORDレコード
- ord-807fcd1429d04fc2b39b3fa6cf263654
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987269B2
反応ノート
読み込み中…