2,2,2-trichloro-1-dimethoxyphosphorylethanol

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In another process, Pesticide Manufacturing and Toxic Materials Control Encyclopedia, edited by Marshall Sittig, Noyes Data Corporation, Park Ridge, N.J. 1980, 75 grams of chloral are dropped into 60 grams of dimethyl phosphite at an initial temperature of 25° C. The temperature slowly rises to 50° C. and is kept at 50° C. to 60° C. by external cooling. After cooling the oil is dissolved in benzene, and the benzene solution is washed with a sodium bicarbonate solution and dried with anhydrous sodium sulfate. After the solvent has been distilled off, an oil is left which is almost completely solidified. After washing with an icy mixture of ether and petroleum ether, the trichloro-α-hydroxyethyl phosphonic dimethyl ester is obtained in the form of colorless needles with a melting point of about 81° C. slowly rises to 50° C. is kept at 50° C. to 60° C. by external cooling After cooling the oil the benzene solution is washed with a sodium bicarbonate solution dried with anhydrous sodium sulfate After the solvent has been distilled off an oil is left which After washing with an icy mixture of ether and petroleum ether

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In another process, Pesticide Manufacturing and Toxic Materials Control Encyclopedia, edited by Marshall Sittig, Noyes Data Corporation, Park Ridge, N.J. 1980, 75 grams of chloral are dropped into 60 grams of dimethyl phosphite at an initial temperature of 25° C. The temperature slowly rises to 50° C. and is kept at 50° C. to 60° C. by external cooling. After cooling the oil is dissolved in benzene, and the benzene solution is washed with a sodium bicarbonate solution and dried with anhydrous sodium sulfate. After the solvent has been distilled off, an oil is left which is almost completely solidified. After washing with an icy mixture of ether and petroleum ether, the trichloro-α-hydroxyethyl phosphonic dimethyl ester is obtained in the form of colorless needles with a melting point of about 81° C. slowly rises to 50° C. is kept at 50° C. to 60° C. by external cooling After cooling the oil the benzene solution is washed with a sodium bicarbonate solution dried with anhydrous sodium sulfate After the solvent has been distilled off an oil is left which After washing with an icy mixture of ether and petroleum ether