SU297643A1 - METHOD OF OBTAINING 0-ALKYL (ARYL) TRITIOPHOSPHATOVKALY - Google Patents

Description

This invention relates to the field of the preparation of salts of thiophosphoric acids, namely O-alkyl (aryl) potassium tritiophosphates.

The above compounds are intermediates for the synthesis of various organophosphorus substances and can be used to produce lubricating oils, flotation agents, surfactants, and insecticides.

A known method for producing potassium O-alkyl (aryl) tritiophosphatB is by reacting phosphorus pentasulfide with an alcohol or phenol in the presence of a tertiary amine, followed by treating the reaction mixture with caustic potash.

The product yield is 40-70%.

In order to increase the product yield, phosphorus ientasulfide is pretreated with sulfur, preferably in an environment of an inert organic solvent, for example benzene, at a temperature of 30-40 ° C.

The desired products are isolated from the reaction mixture by precipitation with acetone. The yield is 52-90%.

Example 1. Getting O.-ethyltritium potassium.

phosphorus pentasulfide and 6.01 g (0.18 mol) of purified sulfur in 70 ml of benzene are heated to 40-50 ° C. To the suspension is added dropwise a mixture of 46.1 ml (0.33 mol) of triethylamine and 9.5 ml (0.17 mol) of ethyl alcohol. The temperature is subsequently maintained within 30-40 ° C. The reaction mass is stirred until complete dissolution of sulfur and phosphorus pentasulfide. Then a methanolic solution of potassium hydroxide is added to the oily layer, the salt is precipitated with acetone.

38.2 g (90.0% of theory) of the product are obtained.

Found,%: S 38.75; 38.88; P 11.72; 11.85.

Calculated,%: S 38,45; R 11.96.

Example 2. Obtaining O-phenyl tritium potassium.

The reaction is carried out under the conditions described above. To a suspension of 18.93 g (0.083 mol) of phosphorus pentasulfide and 6.01 g (0.17 mol) of purified sulfur in 70 ml of benzene, a solution of 15.68 g (0.17 mol) of freshly distilled phenol in 46.1 is added with heating. ml (0.33 mol) of triethylamine until complete dissolution of the suspension is complete. A solution of potassium hydroxide is added to the resulting oil and the salt is precipitated with acetone. The yield of product is 26.0 g (52% of theory).

Example 3. 18.93 g (0.083 mol) of phosphorus pentasulfide, 6.01 g (0.17 mol of sulfur, 46.1 ml (0.33 mol) of triethylamine and 15.2 ml (0.17 mol } absolute butanol. The yield of potassium O-butyltriothiophosphate is 28.4 g (60.3% of theory).

Found,%: S 34.74; 34.87; R 11.00; 10.83.

Calculated,%: S 34,57; R 11.13.

Subject invention

Claims (2)

1. Method for preparing O-alkyl (aryl) potassium tritiophosphates by reacting phosphorus pentasulfide with alcohol or phenol in the presence of a tertiary amine, followed by treating the reaction mixture with caustic potassium and isolating the target product with known methods, in order to increase the yield of the product, phosphorus pentasulfide pretreated with sulfur. 2. A method according to claim 1, characterized in that the treatment of phosphorus pentasulfide with sulfur is carried out in an environment of an inert organic solvent, for example benzene, at a temperature of 30-40 ° C.