Triethyl phosphite → HCID 54111407, compound

Participants

Reaction Steps

252 g of chloromethyl-dimethylphosphine oxide are heated to 140° to 150° C. under an atmosphere of nitrogen and 480 g of triethylphosphite are added dropwise in the course of 4 hours. Stirring is continued for a further 1.5 hours at the temperature indicated, 98 g of ethyl chloride (76% of theoretical) being collected in a cold trap connected downstream of the apparatus. The mixture is then incipiently distilled at 0.6 mm Hg until the internal temperature reaches 148° C., with distillate passing over at a temperature of 135° C. This gives 309 g of the ester, having a solidification point of 59°-60° C. (yield: 68 percent of theoretical). The product can be employed for further reactions in the form of the crude product; further purification can be effected by distillation (boiling point at 0.4 mm Hg: 140° C.).

Provenance & Evidence