Phosphorus pentachloride → HCID 178526581, compound

Participants

Reaction Steps

A mixture of 1 g of 5-hydroxy-3-(o-nitrobenzyl)-1,2,4-triazole, 10 ml of phosphorus oxychloride and 1.89 g of phosphorus pentachloride is stirred at 70° for 11 hours, then at room temperature over the weekend and evaporated to dryness. The residue is dissolved in water, the solution is basified with 10% aqueous potassium carbonate and extracted 3 times with ethyl acetate. The combined extracts are dried over magnesium sulfate, decolorized with charcoal and evaporated to dryness. The residue is chromatographed with 50 g of silica gel using methylene chloride-ethyl acetate (1:1) as eluent to give 5-chloro-3-(o-nitrobenzyl)-1,2,4-triazole, m.p. 160°-163°.

Provenance & Evidence