Diethyl chlorophosphate → HCID 86746781, compound

Participants

Reaction Steps

To a suspension of potassium cyanate (0.82 g, 10.1 mmol) in acetone (10 mL) is added diethyl chlorophosphate (1.3 mL, 9.2 mmol). The mixture is heated at reflux for 90 minutes. After cooling to room temperature, 2,6-diisopropylaniline (1.7 mL, 9.2 mmol) is added. The mixture is stirred at room temperature for 2 hours, then heated at reflux for 2 hours. After cooling, the mixture is filtered. The filtrate is diluted with ethyl acetate, washed twice with brine, dried over magnesium sulfate, and concentrated. Flash chromatography (3:2 ethyl acetate/hexane) provides 1.3 g of the product as a white solid. Recrystallization from ethyl acetate/hexane provides an analytical sample; mp 157°-158° C.

Provenance & Evidence