反应详情

温度

120 °C

Pd(OAc)2 (20 mg, 0.09 mmol, 10%), (±)-BINAP (55 mg, 0.09 mmol, 10%) and dimethylformamide (15 mL) were charged in a round-bottom flask flushed with argon. The mixture was stirred under argon for 30 minutes. Then 3-chloro-p-anisidine (153 mg, 0.97 mmol), 8-iodo-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide (300 mg, 0.84 mmol), K2CO3 (2.45 g, 17.8 mmol) and dimethylformamide (6 mL) were added. The resulting mixture was stirred at room temperature for 1 hour and then heated to 120° C. in an oil bath under argon with good stirring for 18 hours. After cooling to room temperature, the reaction mixture was poured into water (300 mL) and extracted with dichloromethane (5×60 mL). The organic extracts were washed with water (2×20 mL) and dried over anhydrous Na2SO4. The solvent was removed under vacuum, the crude solid was taken up with diethyl ether, filtered, washed with diethyl ether and purified by flash chromatography on silica gel (eluant: dichloromethane/methanol 97.5:2.5) to afford 95 mg of pure title compound.

1. customflushed with argon
2. stirringThe resulting mixture was stirred at room temperature for 1 hour
3. stirringwith good stirring for 18 hours
4. temperatureAfter cooling to room temperature
5. extractionextracted with dichloromethane (5×60 mL)
6. washThe organic extracts were washed with water (2×20 mL)
7. dry with materialdried over anhydrous Na2SO4
8. customThe solvent was removed under vacuum
9. filtrationfiltered
10. washwashed with diethyl ether
11. custompurified by flash chromatography on silica gel (eluant: dichloromethane/methanol 97.5:2.5)