Phosphorus pentachloride → HCID 13144517, compound

Participants

Reaction Steps

3.97 g (0.017 mol) of methyl 2-hydroxymethyl-2,3,5,8-tetrahydro-1,3-dioxo-1H-1,2,4-triazolo[1,2-a]pyridazine-5-carboxylate were suspended at 0° C. in 300 ml of dry ether. 3.49 g (0.017 mol) of phosphorus pentachloride were added portionwise and the mixture was stirred at room temperature for 22 hours. The resulting clear solution was evaporated in vacuo and the residue was chromatographed on silica gel using chloroform/ethyl acetate (1:1) for the elution. There were obtained 3.24 g (76%) of methyl 2-chloromethyl-2,3,5,8-tetrahydro-1,3-dioxo-1H-1,2,4-triazolo[1,2-a]pyridazine-5-carboxylate of melting point 164°-165° C.

Provenance & Evidence