160906-98-9

320405-84-3

160906-98-9

GENERAL PROCEDURE: 2-hydroxy-3-nitropyridine (0.015 mol) was suspended in trichlorophosphorus (15 mL). Anhydrous N,N-dimethylformamide (2 mL) was added and the reaction mixture was heated to reflux for 12 hours. Upon completion of the reaction, the excess phosphorous trichloride was removed by distillation. The residue was dissolved in a mixture of dichloromethane and ice and stirred for 30 minutes. The organic layer was separated, washed three times with water, dried over anhydrous sodium sulfate, filtered and concentrated to give analytically pure 6-chloro-5-nitronicotinonitrile.