反应详情

温度

120 °C

A mixture of 1.7 g of 2-hydroxy-3-nitro-5-(2-methylpropyl)pyridine (starting material D4) and 15 ml of phosphorous oxychloride is heated under reflux to 120° C. for two hours. After cooling the mixture is carefully added to ice/water, then neutralized with sodium-hydrogencarbonate and extracted three times with ethylacetate. The combined organic phases are evaporated to dryness and the residue is chromatographed on a silica gel column (ethylacetate/petroleum ether 1:15). Concentration of the chromatographically pure fractions gives 1.17 g of the title compound as an orange oil.

1. temperatureis heated
2. temperatureAfter cooling the mixture
3. extractionextracted three times with ethylacetate
4. customThe combined organic phases are evaporated to dryness
5. customthe residue is chromatographed on a silica gel column (ethylacetate/petroleum ether 1:15)