Phosphorus oxychloride → HCID 14885582, compound

Participants

Reaction Steps

A solution of 3-[2-(3,4-dichlorophenyl)ethyl]-N-(1,1-dimethylethyl)-2-pyridine carboxamide (37.8 g, 0.107 mole) in 120 mL (197.4 g, 1.29 mole) of phosphorous oxychloride is heated at 110° C. for 4.5 hours. Completion of the reaction is determined by thin-layer chromotography. The reaction is quenched with ice and H2O and the pH of the solution is brought to 8 by the addition of a saturated solution of potassium carbonate. The product is extracted into ethylacetate. The solution is concentrated to a solid residue which upon recrystallization from diethyl ether/ethyl acetate provides the desired product, (27.1 g, 0.098 mole), in 91.6% yield.

Provenance & Evidence