反应详情

2,4-Dichloro-5-fluoropyrimidine (800 mg, 4.8 mmoL), tert-butyl (3-aminophenyl)carbamate (996 mg, 4.8 mmoL) and Hunig's base (948 uL, 5.75 mmoL) were dissolved in THF (20 mL). The reaction mixture was heated at reflux overnight. After cooling, partitioned between water/brine (10 mL), agitated and separated the layers. Dried organic phase over sodium sulfate, and the solvent was removed via rotary evaporation. Titration with EtOAc and Heptane gave after filtration a white solid, 1 g. LC/MS (RT=2.03/(M+1)) 339.1.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. temperatureAfter cooling
4. custompartitioned between water/brine (10 mL)
5. customseparated the layers
6. customDried organic phase over sodium sulfate, and the solvent was removed via rotary evaporation
7. customTitration with EtOAc and Heptane gave
8. filtrationafter filtration a white solid, 1 g
9. customLC/MS (RT=2.03/(M+1)) 339.1