反应详情

温度

70 °C

4-Fluoro-3-nitrophenyl isocyanate (0.45 ml) was added to a solution of (2,2-dimethoxyethyl)-(4-phenoxyphenyl)amine (750 mg) in chloroform (10 ml). The reaction was shaken at 70° C. for 2 hours. A second portion of 4-fluoro-3-nitrophenyl isocyanate (0.45 ml) was added. After 16 hours at 70° C., volatiles were removed and TFA.(10 ml) was added. After shaking for 16 hours, volatiles were removed and the residue was purified by chromatography on silica gel (eluent: dichloromethane/hexane 8:1). The product with the molecular weight of 391.36 (C21 H14FN3O4); MS (ESI): 392 ([M+H]+), was obtained in this way.

1. waitAfter 16 hours at 70° C.
2. customvolatiles were removed
3. addition(10 ml) was added
4. stirringAfter shaking for 16 hours
5. customvolatiles were removed
6. customthe residue was purified by chromatography on silica gel (eluent: dichloromethane/hexane 8:1)
7. customMS (ESI): 392 ([M+H]+), was obtained in this way