Phosphorus oxychloride → HCID 21882743, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1.6 g of 5-(3,4-dichlorphenyl)-2-hydroxy-3-nitropyridine (starting material G4) and 10 ml of phosphorous oxychloride is heated under reflux to 120° C. for 3 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 1:20). Concentration of the chromatographically pure fractions gives 0.88 g of the title compound as yellow crystals. The mass spectrum shows the molecular peak M+ at 302 Da.

Provenance & Evidence