反应详情

温度

0 °C

In a 125 mL round-bottom flask, 3-morpholinophenol (0.91 g, 5.07 mmol) was dissolved in THF (40 mL). Solution was cooled to 0° C. and NaHMDS (5.07 mL, 5.07 mmol) (1M in THF) was added slowly. The mixture was agitated for 15 minutes and solution of 3-fluoro-2-nitropyridine (0.60 g, 4.22 mmol) in THF (5 mL) was added slowly. After agitating for 2 hours the solvent was evaporated and the residue dissolved in 100 mL of CH2Cl2 and washed with diluted sodium bicarbonate solution twice, dried over magnesium sulfate, filtered and evaporated. Crude material was purified by chromatography on silica gel, eluted with 25% ethyl acetate/Hexane to give the title compound (0.93 g, 72%) was obtained as thick red oil.

1. stirringAfter agitating for 2 hours the solvent
2. customwas evaporated
3. dissolutionthe residue dissolved in 100 mL of CH2Cl2
4. washwashed with diluted sodium bicarbonate solution twice
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customCrude material was purified by chromatography on silica gel
9. washeluted with 25% ethyl acetate/Hexane