反应详情

温度

120 °C

To a stirred solution of 2-methyl-5-fluoro-quinazoline (WO2003068772, Chem. Abstr. 139:197493, 2 g; 12.3 mmol) in dry dimethylformamide (10 mL) were added triethylamine (3.4 mL; 2 eq) and piperazine (11 g; 10 eq). The reaction mixture was stirred under nitrogen at 120° C. for 4 h, then cooled to room temperature, poured into water (10 mL) and extracted with ethyl acetate (5×15 mL). The organic layers were combined, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by ion-exchange chromatography [SCX-2; MeOH—1M NH3/MeOH (1:0)→(0:1)] to afford the title compound as a yellow solid (1.8 g; yield 64%).

1. temperaturecooled to room temperature
2. extractionextracted with ethyl acetate (5×15 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by ion-exchange chromatography [SCX-2; MeOH—1M NH3/MeOH (1:0)→(0:1)]