Chloroacetonitrile → ethyl (cyanomethyl)methylphosphinate

Participants

Reaction Conditions

Reaction Steps

226.5 g (3 mol) of chloroacetonitrile were heated to 60° C. 470 g (3.53 mol) of diethyl methylphosphonate were added dropwise over a period of 3 hours at 70° to 80° C. During this step heating was not necessary; the reaction was exothermic. Ethyl chloride was collected in a down-stream cold trap. After the dropwise addition was finished, the mixture was slowly heated to 125° C. and kept at this temperature until no more waste gas (ethyl chloride) could be detected. The mixture was subsequently cooled and distilled through a column under an aspirator vacuum to give 418 g of ethyl cyanomethtylmethylphosphinate (b.p. 108°-109° C., 0.0133 kPa). This correspnds to a yield of 95% of theory, based on the amount of chloroacetonitrile used. ##STR4##

Provenance & Evidence