反应详情

温度

25 °C

To a stirred suspension of sodium hydride (2 g) in dry tetrahydrofuran (25 mL) under a nitrogen atmosphere was added a solution of methyl 2-amino-5-methylthiophene-3-carboxy-late (4.8 g, 0.028 mol) and 2-fluoronitrobenzene (4.0 g, 0.025 mol) in dry tetrahydrofuran (30 mL). The mixture was stirred at 25° C. for 20 hours, poured onto ice and partitioned between 2N hydrochloric acid and ethyl acetate. The organic extracts were dried over magnesium sulfate, the solvent was evaporated under reduced pressure and the title compound purified by chromatography on silica gel, eluted with toluene, and crystallized from ethanol (4.1 g).

1. additionpoured onto ice
2. custompartitioned between 2N hydrochloric acid and ethyl acetate
3. dry with materialThe organic extracts were dried over magnesium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customthe title compound purified by chromatography on silica gel
6. washeluted with toluene
7. customcrystallized from ethanol (4.1 g)