反应详情

温度

150 °C

Tert-butyl (1-(4-fluoro-3-nitrophenyl)ethyl)carbamate (500 g, 1.75 mmol) was stirred in THF (2 ml). NH4OH (0.978 ml, 7.0 mmol) was added and the reaction mixture was heated at 150° C. for 30 minutes using microwave (Biotage Initiator). NH4OH (0.6 00 ml) was added and then heated at 180° C. After cooling to room temperature, the reaction mixture was poured into EtOAc/water. The organic layer was washed with brine, dried over MgSO4 and evaporated. The resulting material was purified by flash chromatography on silica eluting with 0% to 50% EtOAc/Hexane to afford the title compound (376 mg, yield: 76%) 1H-NMR (400 MHz, CDCl3) δ 1.43-1.48 (m, 12H) 4.71 (br. s., 2H) 6.79 (d, 1H) 7.34 (dd, 1H) 8.05 (d, 1H).

1. temperatureheated at 180° C
2. temperatureAfter cooling to room temperature
3. washThe organic layer was washed with brine
4. dry with materialdried over MgSO4
5. customevaporated
6. customThe resulting material was purified by flash chromatography on silica eluting with 0% to 50% EtOAc/Hexane