p-Fluoronitrobenzene → HCID 21105671、化合物
反応式
[CH3:1][NH:2][CH:3]1[CH2:7][CH2:6][NH:5][CH2:4]1.F[C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=1>>[CH3:1][NH:2][CH:3]1[CH2:7][CH2:6][N:5]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=2)[CH2:4]1参加物
3
反応条件
- 温度
- 110 °C
実験手順
N-methylpyrrolidin-3-amine (0.788 g, 7.87 mmol) was added to 1-fluoro-4-nitrobenzene (1.11 g, 7.87 mmol) slowly (CAUTION: extreme exotherm!!!). The resulting mixture was heated at 110° C. for 10 min. After cooling down to room temperature, another portion of amine (0.156 g) was added to the reaction mixture. The resulting mixture was heated at 110° C. for 1 h. After cooling down to room temperature, the obtained black solid product (Example 43A) was used for next step without further purification. LCMS (ES): m/z 252.3 [M+H]+.
後処理
- temperatureAfter cooling down to room temperature
- temperatureThe resulting mixture was heated at 110° C. for 1 h