反应详情

A stirred partial solution of 4-chloro-5-fluoroquinazoline (10.95 g, 60 mmol) and 5-aminoindazole (7.98 g, 60 mmol) in isopropanol (300 ml) was heated under reflux for 3 hours. On cooling to ambient temperature the product hydrochloride salt was filtered off and washed with isopropanol and ether. The salt was heated with water (400 ml)/ethanol (100 ml) and the partial solution was basified with aqueous ammonia. The precipitated solid was filtered off and washed with water to provide 5-fluoro-N-1H-indazol-5-ylquinazolin-4-amine (14.91 g, 89%); NMR spectrum (300 MHz) 7.42 (dd, 1H), 7.53 (s, 2H), 7.60 (d, 1H), 7.83 (m, 1H), 8.08 (d, 2H), 8.50 (s, 1H), 9.20 (d, 1H), 13.05 (s, 1H); Mass spectrum MH+ 280.

1. temperatureunder reflux for 3 hours
2. filtrationwas filtered off
3. washwashed with isopropanol and ether
4. temperatureThe salt was heated with water (400 ml)/ethanol (100 ml)
5. filtrationThe precipitated solid was filtered off
6. washwashed with water