Phosphoric acid (bis)di:methylamide (di)chloride prodn. - by reaction of di:methylamine with phosphorus oxychloride; used as pesticide intermediates

摘要

In a new process for the prodn. of phosphoric acid dimethylamide dichloride (I) or phosphoric acid bis(dimethylamide) monochloride (II) by reaction of dimethylamine with a stoichiometric amt. of POCl3 under anhydrous conditions, (A) the dimethylamine is added to a mixt. of POCl3 and the desired reaction prod. as reaction medium, and (B) (I) or (II) is opt. subsequently sepd. from dimethylammonium chloride formed as byprod. and purified in a known manner by distn. Pref., (I) or (II) is used as solvent in an amt. of 0.5-1 mol per mol of dimethylammonium chloride form as byprod. In the prodn. of (I), dimethylamine is pref. used in a total amt. of 2 mol per mol POCl3 and is pref. added at such a rate that the reaction temp. does not exceed 110 deg.C. In the prodn. of (II), dimethylamine is pref. used in a total amt. of 4 mol per mol POCl3 and is pref. added at such a rate that the reaction temp. does not exceed 170 deg.C. (I) and (II) are useful as intermediates for pesticides, solvents and lubricants. The proceeds proceeds with good yields and good selectivity, without the need for intensive cooling or for distn. of large amts. of solvents.