Formic Acid → HCID 20283629, Verbindung

A reaction mixture consisting of 2,2-dichloroacetamide (6.4 g, 50 mmol), phosphorus pentachloride (10.4 g, 50 mmol), and carbon tetrachloride (50 mL) was stirred under nitrogen while heated at reflux for 30 minutes. A clear solution resulted, which was cooled to room temperature. Formic acid (1.9 mL, 50 mmol) was added dropwise with stirring, and formation of a white precipitate was observed. The stirring was continued for 1 hour at ambient temperature. The white solid was separated by filtration, rinsed with carbon tetrachloride, and dried in vacuum over phosphorus pentoxide at ambient temperature. A yield of 10 g (82%) of N-(dichlorophosphinyl)-2,2-dichloroacetamide was obtained.