反应详情

温度

0 °C

To a solution of 7-bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazoline (2.80 g) in N,N-dimethylformamide (56 ml) was added sodium hydride (60% in mineral oil, 334 mg) with stirring at 0° C. under an atmosphere of nitrogen and the mixture was stirred at room temperature for 1 hour. To this mixture was added ethyl bromoacetate (0.85 ml) dropwise and the mixture was stirred at room temperature for 2 hours. The solvent was removed under reduced pressure to give a residue, which was poured into water and extracted with ethyl acetate. The extract was washed with water and dried. Removal of the solvent followed by recrystallization from isopropyl either gave ethyl 2-[7-bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetate (3.11 g).

1. stirringthe mixture was stirred at room temperature for 1 hour
2. stirringthe mixture was stirred at room temperature for 2 hours
3. customThe solvent was removed under reduced pressure
4. customto give a residue, which
5. extractionextracted with ethyl acetate
6. washThe extract was washed with water
7. customdried
8. customRemoval of the solvent
9. customfollowed by recrystallization from isopropyl