Phosphorus oxychloride → HCID 21882749, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1.8 g of 2-hydroxy-3-nitro-5-cyclohexylmethylpyridine (starting material E4) and 13 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 ethyl acetate. 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 0.84 g of the title compound as an orange oil.

Provenance & Evidence