SU202129A1 - METHOD OF OBTAINING ALKYDIALCOXYPHOSPHOSOCIANS - Google Patents

Description

The invention relates to methods for producing phosphazocyanoB, which can be used as intermediates - in the synthesis of dohimikatov, drugs, etc.

A method is proposed for the preparation of the alkyl dialkoxyphosphazocyanes of the general formula

OR

RP NCN, R and R - alkyl based on OR

the interaction of dialkyl esters of alkylphosphonic acids with cyanazide in a solution of acetonitrile at 5-15 ° C. The non-distilled alkyl dialkoxyphosphazocyanes are analytically pure individual substances. In the process of distillation, even in a deep vacuum, they undergo a regrouping.

Example. In a four-necked flask equipped with a stirrer, a thermometer, a bubbler, dipped to the bottom, and a reflux condenser, 40-50 ml of absolute acetonitrile and 0.1 gmol of activated sodium azide are placed. Under stirring, 0.05 g-mol of dry chlorocyanum is passed into the reaction mixture so that the temperature of the mixture does not exceed 10-12 ° C (external cooling). At the end of the passage of chlorine cyan, the temperature of the reaction mass is brought to room temperature, without stopping stirring. The precipitate is filtered off.

While stirring, a filter containing cyanazide was added dropwise with 0.051 g-mol of alkylphosphinic acid dialkyl ester with

at a rate such that the temperature of the reaction mass does not exceed 15 ° C (external cooling). The temperature of the reaction mass is brought to room temperature, the solvent is distilled off in vacuum. Balance (in case of

in it solid particles are filtered) kept in vacuum 0.02 mm Hg. Art. at room temperature 4 hours and at 50 ° C for another 1 hour.

Methyldiethoxyphosphazocyan. 75% yield;

OA9L

df 1.1114; 1.4601 each.

Found,%: C 41.75; H 7.07;

N 15.73; P 16.52; HOW 50,55. MR 43.36. C, H ,, N-20-2P.

N 15.9;

Calculated,%: C 40.9; H 7.38; P 17.61; SzNzO 51.1; MR 43.25. Mol weight: calculated 176, found 170,174. Methyldipropoxyphosphazocyan. Yield 80%; df 1.0712; 1.4605. Found,%: C 47.07; H 8.97; N 13.45; R 15.56; CzNtoO 56,23, -MR 52,16. CgHivNgOa. Calculated,%: C 47.05; H 8.33; N 13.72; R 15.19; CzNtoO 58.3, MR 52.49. Mol weight: calculated 204, found 212,206. Methyldibutoxyphosphazotsnan. Yield 82%; df 1.0289; 1.4606 each. tol N 12,11; Found,%: C 50.81; H 9.19; R 12.91; CiHgO 64.28, MR 61.80. CioHsiNaOaP. Calculated,%: C 51.72; H 9.05; N 12.06; R 13.36; CiHgO 63; MR 61.73. Mol weight: calculated 232; found 235.225. Subject of the invention 1. A method for producing alkyl dialkoxyphosphazocyanes, characterized in that the dialkyl esters of alkylphosphinic acids are treated with cnanazide in an acetonitrile solution under cooling. 2. A method according to claim 1, characterized in that the cooling is carried out to 5-15 ° C.