反应详情

5-Benzoyl-6-(bromomethyl)-1,3-dimethylpyrimidine-2,4(1H,3H)-dione (Intermediate C) (1.15 g, 3.41 mmol), benzyl carbazate (commercial) (2.83 g, 17.05 mmol) and triethylamine (1.426 ml, 10.23 mmol) were combined in EtOH (15 ml) and the mixture heated at reflux for 15 mins. The reaction mixture was cooled to RT and evaporated under reduced pressure. The residue was partitioned between water and DCM and the phases separated. The organic phase was passed through a hydrophobic frit and evaporated under reduced pressure. The residue was triturated with Et2O and cooled in ice until precipitation occurred. The precipitate was collected by filtration, affording the title compound as a white solid.

1. temperaturethe mixture heated
2. temperatureat reflux for 15 mins
3. customevaporated under reduced pressure
4. customThe residue was partitioned between water and DCM
5. customthe phases separated
6. customevaporated under reduced pressure
7. customThe residue was triturated with Et2O
8. temperaturecooled in ice until precipitation
9. filtrationThe precipitate was collected by filtration