反应详情

2-Amino-6-fluorobenzamide (77 mg, 0.50 mmol) was dissolved under argon in dimethylacetamide (5 ml), 4-bromo-1H-pyrazole-5-carbaldehyde (88 mg, 0.50 mmol) and Na2S2O5 (143 mg, 0.75 mmol) were added, and the mixture was stirred under reflux conditions for 5 h. After cooling to room temperature, the reaction mixture was concentrated and taken up with a mixture of acetonitrile and N,N-dimethylformamide. Filtration with suction and thorough drying of the remaining solid gave 2-(4-bromo-1H-pyrazol-5-yl)-5-fluoroquinazolin-4(3H)-one (30 mg, 19% of theory) as a colorless solid. 1H NMR (400 MHz, d6-DMSO δ, ppm) 13.91 (br. s, 1H, NH), 12.03 (br. s, 1H, NH), 8.22 (s, 1H), 7.80 (dd, 1H), 7.51 (d, 1H), 7.27 (dd, 1H).

1. concentrationthe reaction mixture was concentrated
2. additiontaken up with a mixture of acetonitrile and N,N-dimethylformamide
3. filtrationFiltration with suction
4. customthorough drying of the remaining solid