Ammonia → HCID 84079540、化合物
反応式
C[O:2][C:3](=O)[NH:4][CH2:5][CH:6]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=1)[CH3:7].N>>[Cl:14][C:10]1[CH:9]=[C:8]2[C:13](=[CH:12][CH:11]=1)[C:3](=[O:2])[NH:4][CH2:5][CH:6]2[CH3:7]参加物
3
反応条件
- 温度
- 120 °C
実験手順
Under N2 protection, a mixture of [2-(3-chloro-phenyl)-propyl]-carbamic acid methyl ester (3.0 g, 13.2 mmol) and PPA (polyphosphoric acid) (10 g) in a 100 mL flask was stirred at 120° C. for 2 hours. After cooling to room temperature, the reaction mixture was treated with ice-water and aqueous ammonia solution to adjust the pH to 8. The mixture was extracted with EtOAc, and the organic layer was washed with brine, dried over anhy. Na2SO4, filtered and concentrated in vacuo. The crude product formed was further washed with ether to give the title compound (0.52 g, 20%) as a white solid. MS: 196.1 (M+H+).
後処理
- temperatureAfter cooling to room temperature