反应详情

To a 10 mL microwave reaction flask reaction charged with a magnetic stir bar, was added 2-chloro-5-[5-(3-chlorothiophene-2-yl)-[1,2,4]oxadiazol-3-yl]-phenylamine (0.100 g, 0.320 mmol), anhydrous ethanol (1.3 mL), bromo ethylacetate (0.241 g, 1.44 mmol) and triethylamine (67 μL, 0.48 mmol). The suspension was reacted at 120° C., for 15 min in a microwave set at 70 watts. The resulting yellow suspension was diluted with ethyl acetate (50 mL) and the organic layer was then washed with H2O (2×15 mL), brine (10 mL), dried over MgSO4, and the solvent was removed by evaporation. The white solid was then purified by flash column chromatography (silica gel, elution with EtOAc:hexanes, 1:5) to yield 0.119 g (94%) of the title compound as a white solid. 1H NMR (CDCl3): 7.59 (dd, 1H, J=5.2 and 1.4 Hz), 7.47 (dd, 1H, J=8.3 and 1.7 Hz), 7.38 (dd, 1H, J=8.3 and 1.1 Hz), 7.27 (d, 1H, J=1.7 Hz), 7.10 (dd, 1H, J=5.2 and 1.4 Hz), 5.11 (t, 1H, J=5.0 Hz), 4.29 (q, 2H, J=7.1 Hz), 4.05 (d, 2H, J=5.2 Hz), 1.33 (t, 3H, J=7.1 Hz).

1. customTo a 10 mL microwave reaction flask reaction
2. additioncharged with a magnetic stir bar
3. customThe suspension was reacted at 120° C., for 15 min in a microwave
4. washthe organic layer was then washed with H2O (2×15 mL), brine (10 mL)
5. dry with materialdried over MgSO4
6. customthe solvent was removed by evaporation
7. customThe white solid was then purified by flash column chromatography (silica gel, elution with EtOAc:hexanes, 1:5)