Methyl iodide → Diethyl methylphosphonate

Participants

Reaction Conditions

Reaction Steps

188 g (1.32 mol) of methyl iodide are poured under nitrogen into a dry three-necked flask surmounted by an alcohol condenser (-10° C.), and then heated to the refluxing temperature. 168 g (1.02 mol) of triethyl phosphite are then added dropwise. The reaction is exothermic, and the temperature rises in the course of one hour to 73° C. The temperature of the mixture is maintained for one hour at between 70° and 75° C., and the solution is then cooled and concentrated in a rotary evaporator. The diethyl methylphosphonate is distilled under nitrogen, under reduced pressure.

Provenance & Evidence