反应详情

0.5 g of 2-chloro-5-nitro-pyridine (3.15 mmol), 1.2 g of tributyl-vinyl-stannane (3.78 mmol), 0.036 g of tetrakistriphenylphosphinpalladium(0) (0.03 mmol), and 0.024 g of triphenylphosphin (0.09 mmol) were dissolved in 20 ml of toluene and stirred for 2 h under reflux. Upon cooling to room temperature, 10 ml of water were added, the aqueous layer was extracted with ethyl acetate, and the combined organic layers were washed with saturated sodium chloride, dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure. The crude product was purified via silica gel chromatography with cyclohexane/ethyl acetate (10%). Fractions containing the product were combined, the solvent evaporated to yield 0.528 g of the desired product.

1. temperatureunder reflux
2. extractionthe aqueous layer was extracted with ethyl acetate
3. washthe combined organic layers were washed with saturated sodium chloride
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customthe solvent evaporated under reduced pressure
7. customThe crude product was purified via silica gel chromatography with cyclohexane/ethyl acetate (10%)
8. additionFractions containing the product
9. customthe solvent evaporated