反应详情

温度

25 °C

To a stirred slurry of sodium hydride (14.4 g, 50% dispersion in oil, 0.3 mol) in dry tetrahydrofuran (50 mL) under nitrogen was added, dropwise, a solution of 2-fluoro-nitrobenzene (28.2 g, 0.2 mol) and 2-amino-5- methylthiophene-3-carbonitrile (27.6 g, 0.2 mol) in dry tetrahydrofuran (250 mL). The mixture was stirred at 25° C. for 24 hours, poured onto cracked ice and extracted into dichloromethane (3×500 mL). The combined extracts were washed with 2N hydrochloric acid (2 ×200 mL), water (2×200 mL), dried over magnesium sulfate and the solvent removed under reduced pressure. The residue was crystallized from ethanol to give the title compound, (35.2 g), m.p. 99°-102° C.

1. additionpoured
2. extractionextracted into dichloromethane (3×500 mL)
3. washThe combined extracts were washed with 2N hydrochloric acid (2 ×200 mL), water (2×200 mL)
4. dry with materialdried over magnesium sulfate
5. customthe solvent removed under reduced pressure
6. customThe residue was crystallized from ethanol