Dibromomethane → 1-[Ethoxy(isothiocyanato)phosphoryl]oxyethane

Participants

Reaction Steps

To a stirred slurry of 1.0 to 1.2 molar equivalent of anhydrous sodium-, potassium- or ammonium thiocyanate in about 50 ml to 100 ml of a solvent, such as benzene, toluene, xylene, ethylene dichloride, chloroform, methylene chloride and methylene bromide, one molar equivalent of diethoxyphosphoryl chloride of formula (II) is added at a temperature range of 5° to 30° C and, preferably, from 15° to 25° C, while stirring for a period of time from 2 to 4 hours to yield diethoxyphosphinyl isothiocyanate of formula (III). The reaction is slightly exothermic, and controlled by either adjusting the rate of addition of said phosphoryl chloride or employing a cooling bath or even using both.

Provenance & Evidence