反应详情

A mixture of 5-methoxy-N-[1-(pyridin-2-ylmethyl)-1H-indazol-5-yl]quinazolin-4-amine (10.1 g, 27.4 mmol) and pyridine hydrochloride (15.8 g, 137 mmol) in pyridine (150 ml) was heated at reflux for 3 hours. After cooling and evaporation of the solvents, the residue was triturated in 5% aqueous sodium bicarbonate and the resulting mixture was stirred for 30 minutes. The yellowish precipitate was filtered, washed with water and ether, and dried over P2O5 under high vacuum to give 4-{[1-(pyridin-2-ylmethyl)-1H-indazol-5-yl]amino}quinazolin-5-ol as a solid (10.1 g, 100%); NMR spectrum 5.76 (s, 2H), 6.67 (m, 2H), 6.96 (d, 1H), 7.29 (m, 1H), 7.42 (m, 1H), 7.52 (dd, 1H), 7.74-7.66 (m, 2H), 8.13 (s, 1H), 8.33 (s, 2H), 8.52 (d, 1H); Mass spectrum MH+ 369.

1. temperaturewas heated
2. temperatureat reflux for 3 hours
3. temperatureAfter cooling
4. customevaporation of the solvents
5. customthe residue was triturated in 5% aqueous sodium bicarbonate
6. filtrationThe yellowish precipitate was filtered
7. washwashed with water and ether
8. dry with materialdried over P2O5 under high vacuum