反应详情

To a solution of 5-bromonicotinic acid (20.0 g, 99.0 mmol) in ethanol (300 mL) was added DPPA (21.6 mL, 100.0 mmol) followed by triethylamine (14.3 mL, 103.0 mmol) then refluxed overnight. After cooling, a half amount of solvent was removed by evaporation. The ethanol solution was extracted with ethyl acetate. The organic layer was washed with NaHCO3 (aq) and brine, dried over Na2SO4 then evaporated. Sequence purification on SiO2 column chromatography gave the title compound (4.55 g, 19%): MS m/e 245, 246 (M+1).

1. temperaturethen refluxed overnight
2. temperatureAfter cooling
3. customa half amount of solvent was removed by evaporation
4. extractionThe ethanol solution was extracted with ethyl acetate
5. washThe organic layer was washed with NaHCO3 (aq) and brine
6. dry with materialdried over Na2SO4
7. customthen evaporated
8. customSequence purification on SiO2 column chromatography