反应详情

温度

50 °C

A mixture of 3-(2,4-dimethoxybenzyl)-6-ethylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (2 g), 4′-(bromomethyl)-2′-fluorobiphenyl-2-carbonitrile (2 g), potassium carbonate (1.6 g) and acetonitrile (40 mL) was stirred at 50° C. for 1.5 hr. Insoluble material was filtered off, and the solvent was evaporated under reduced pressure. The obtained residue was dissolved in trifluoroacetic acid (15 mL), and the mixture was stirred at 50° C. for 2 hr. The reaction mixture was concentrated under reduced pressure. To the obtained residue was added ethyl acetate, and insoluble material was filtered off. The filtrate was concentrated and recrystallized from diethyl ether to give the title compound as a colorless solid (1.6 g, 90%).

1. filtrationInsoluble material was filtered off
2. customthe solvent was evaporated under reduced pressure
3. dissolutionThe obtained residue was dissolved in trifluoroacetic acid (15 mL)
4. stirringthe mixture was stirred at 50° C. for 2 hr
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. additionTo the obtained residue was added ethyl acetate, and insoluble material
7. filtrationwas filtered off
8. concentrationThe filtrate was concentrated
9. customrecrystallized from diethyl ether