反应详情

A mixture of 7-benzyloxy-6-methoxy-4-(2,3-methylenedioxyanilino)quinazoline hydrochloride (21 g), ammonium formate (30.2 g), 10% palladium-on-charcoal catalyst (4.8 g), water (26 ml) and DMF (350 ml) was stirred at ambient temperature for 2 hours. The mixture was filtered and the filtrate was evaporated. The residual oil was triturated under diethyl ether. The solid so obtained was triturated under water, collected by filtration, washed with water and with diethyl ether and dried under vacuum over phosphorus pentoxide. The material so obtained was purified by column chromatography on silica using a 9:1 mixture of methylene chloride and methanol as eluent. There was thus obtained the title compound (15 g); NMR Spectrum: (DMSOd6) 3.95 (s, 3H), 6.0 (s, 2H), 6.85 (m, 2H), 6.95 (d, 1H), 7.05 (s, 1H), 7.8 (s, 1H), 8.3 (s, 1H), 9.4 (s, 1H), 10.3 (s, 1H); Mass Spectrum: M+H+ 312.

1. filtrationThe mixture was filtered
2. customthe filtrate was evaporated
3. customThe residual oil was triturated under diethyl ether
4. customThe solid so obtained
5. customwas triturated under water
6. filtrationcollected by filtration
7. washwashed with water and with diethyl ether
8. dry with materialdried under vacuum over phosphorus pentoxide
9. customThe material so obtained
10. customwas purified by column chromatography on silica using
11. additiona 9:1 mixture of methylene chloride and methanol as eluent