反应详情

After dissolving 5.86 g of the crude 3-tert-butoxy-5-chloropyrazine-2-carboxaldehyde in 55 ml of acetonitrile, 4.77 g of potassium fluoride, 1.13 g of tetraphenylphosphonium bromide and 0.71 g of 18-crown-6 were added and the mixture was heated to reflux for 4 hours. Diethyl ether was added to the reaction mixture, the insoluble portion was filtered out, and the filtrate was distilled off under reduced pressure. Ethyl acetate was added to the residue, the insoluble portion was filtered out, and the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: toluene/ethyl acetate) to obtain the title compound (183 mg, 3% yield).

1. additionwere added
2. temperaturethe mixture was heated
3. temperatureto reflux for 4 hours
4. filtrationthe insoluble portion was filtered out
5. distillationthe filtrate was distilled off under reduced pressure
6. additionEthyl acetate was added to the residue
7. filtrationthe insoluble portion was filtered out
8. distillationthe filtrate was distilled off under reduced pressure
9. customThe residue was purified by silica gel column chromatography (solvent: toluene/ethyl acetate)