反应详情

温度

80 °C

0.21 mL (1.8 mmol) of n-pentylamine is added to a solution of 0.45 g (0.9 mmol) of ethyl (Z)-2-ethoxy-3-(4-{6-[methyl-(4-nitrophenoxycarbonyl)amino]pyrid-2-yl}phenyl)acrylate (prepared according to Example 2d) in 15 mL of dimethylformamide. The tube is sealed and rapidly placed in an oil bath preheated to 80° C. The reaction mixture is stirred at 80° C. for 1 hour 30 minutes. After cooling, the reaction is worked up by addition of 10 mL of water and extraction with ethyl acetate. The organic phases are combined, washed with saturated aqueous sodium chloride solution and then dried over magnesium sulfate. The solvents are evaporated off. The crude product obtained is purified by chromatography on a column of silica eluted with a 70/30 heptane/ethyl acetate mixture to give 0.2 g (57%) of ethyl (Z)-2-ethoxy-3-{4-[6-(1-methyl-3-pentylureido)pyrid-2-yl]phenyl}acrylate in the form of a pale yellow solid.

1. customThe tube is sealed
2. customrapidly placed in an oil bath
3. custompreheated to 80° C
4. temperatureAfter cooling
5. washwashed with saturated aqueous sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. customThe solvents are evaporated off
8. customThe crude product obtained
9. customis purified by chromatography on a column of silica
10. washeluted with a 70/30 heptane/ethyl acetate mixture