反应详情

温度

95 °C

A mixture of 4-(6-chloro-2,3-methylenedioxyanilino)-7-hydroxy-5-(N-methylpiperidin-4-yloxy)quinazoline (0.1 g), 2,2,2-trifluoroethyl 4-toluenesulphonate (0.071 g), potassium carbonate (0.08 g) and DMF (2 ml) was stirred and heated to 95° C. for 24 hours. The mixture was cooled to ambient temperature and partitioned between ethyl acetate and water. The organic solution was washed with water and with brine, dried over magnesium sulphate and evaporated The residue was purified by column chromatography on silica using a 45:46:4 mixture of methylene chloride, ethyl acetate and methanol as eluent. There was thus obtained the title compound (0.058 g); NMR Spectrum: (CDCl3) 1.95–2.1 (m, 2H), 2.1–2.3 (m, 2H), 2.32 (s, 3H), 2.3–2.45 (m, 2H), 2.75 (m, 2H), 4.48 (m, 2H), 4.64 (m, 1H), 6.05 (s, 2H), 6.6 (d, 1H), 6.74 (d, 1H), 6.78 (d, 1H), 6.97 (d, 1H), 8.5 (s, 1H), 9.28 (s, 1H); Mass Spectrum: M+H+ 511 and 513.

1. temperatureThe mixture was cooled to ambient temperature
2. custompartitioned between ethyl acetate and water
3. washThe organic solution was washed with water and with brine
4. dry with materialdried over magnesium sulphate
5. customevaporated The residue
6. customwas purified by column chromatography on silica using
7. additiona 45:46:4 mixture of methylene chloride, ethyl acetate and methanol as eluent