Acetyl chloride → DIMETHYL ACETYLPHOSPHONATE

Participants

Reaction Steps

Trimethyl phosphite (57.1 g, 0.46 mol) is added dropwise to an ice cold solution of acetyl chloride (36.2, 0.26 nol) at a rate that the internal temperature did not rise above 5° C. The ice bath is removed and the solution warmed to room temperature and then heated to 100° C. for 1 hour. The solution is then vacuum distilled through a 12-inch Vigeraux column to give 30.87 g, 44% of a clear liquid with bp 57°-60° C. at 0.5 mm. H and C nmr are consistent with the assigned structure. This procedure is adapted from the published method of McConnell, R. L., Coover, H. W.,Jr. J. Am. Chem. Soc., 1956, 78, 4450-4452. ##STR20##

Provenance & Evidence