SU515747A1 - Derivatives of dithiopyril with the complexing ability to precious and non-ferrous metals - Google Patents

Description

An amount of 100 g is dissolved in a reaction flask in 300 ml of water and an excess of 10% solution (10-fold excess) of potassium hydrosulfide is poured with stirring in small portions. Rea.ktsi goes very rapidly with the release of hydrogen sulfide. The resulting mixture is heated in a water bath and kept at 70 ° C for 1 hour. The solution is cooled and the precipitated mass of dithiopyrylmethane is separated by filtration under vacuum. The resulting product is recrystallized from ethanol, and then from acetic acid. The precipitate is dried under vacuum. Dithio-1PyrylMetane is obtained as a white crystalline product.

Yield 73 g; t. 1il 237 ° C.

Found,%: C 65.53; H 5.65; N 13.42; iS 16.23.

| Calcd.,%: C 65.70; H 5.70; N 13.37;

516.25.

Example 2. Getting methyldithiophenylmethane. A mixture of 75 g of methyldianthipyrylmethane and 120 ml of phosphorus oxychloride is heated in a reaction flask in an oil bath at an oil bath temperature of 145 ° C for

6 hours with continuous stirring of the reaction mass. (After that, excess oxychloride / phosphorus is distilled off under reduced pressure and a temperature of 95 ° C. The resulting substance, methyldichloropyril metats, is dissolved in hot water and recrystallized first from water and then from 200 ml of alcohol.

| You: CHO methyldichloropyrilmethane 67 g; m. 219 ° C

Paideno,%: C 56.33; P 5,10; N 11.22; C1 27.68.

calculated%; C, 66.23; H 5.08; N 10.93; C1 27.76.

The resulting methyldianthipyrylmethane chloride in an amount of 60 g is processed by heating in a bipolar water bath in an excess of a 10% solution of potassium hydrosulfide. After termination of the reaction, the resulting compound is filtered, washed with water from an excess of potassium hydrosulfide, dried and recrystallized from acetic acid.

Methyldithiophenylmethane is obtained.

Yield 32 g; tl 255 ° C.

Found,% C 66.44; H 5.82;

N 13.16; S 14.90.

Calculated,%: C, 66.36; H 5.99; N 12.90; S 14.98.

Example 3. Getting

IMAGE TILDYTHYPYRYLMETHANE.

In a three-necked flask with a capacity of 600 lgl, equipped with an inverse refrigerator, a thermometer, a stirrer, loaded 200 g of isobutyldianthipyrylmethane. Then, with stirring, 400 ml of pure is added via a dropping funnel in small lorcia. The isobutyldianthipyrylmethane is heated to complete dissolution at a mixture temperature in the reaction flask at 110 ° C and the mixture is kept for 10 hours. P1 excess of phosphorus oxychloride is distilled off in vacuum, destroying oxychlorides with water. The resulting isobutyldianthipyrylmethane chloride is recrystallized and then treated while it is boiled with a solution of potassium hydrosulfide until the reaction is complete. Psobutyldithiophenylmethane is recrystallized.

(Yield 92 g, t. Pl. 259 ° C.

Found,%: C 67.90; H 6.78; N 11.62 S 15.62.

Calculated,%: C 68.07; H 6.72; N 11.76; S 16.44.

iB. Acidic solutions. The derivatives of dithiopyrylmethane form intensely colored complex cationic compounds, of which dithiopyrylmethane (DTM) is of the greatest interest. DTM provides analytically valuable products with bismuth, gold, tellurium, molybdenum. Characteristics of the resulting metal ion compounds with DTM are presented in the table:

Dietary polymer and its derivatives do not absorb in the visible region of the spectrum and form complexed complex compounds with many elements that have an adsorption maximum in the dipole zone for waves 360-560 ° log.

with high values of molar occlusion coefficients. Do not form colored compounds alkaline, alkaline-earth, rare-earth, lead, cadmium, cob

balls, aluminum, zinc, platinum, osmium, mar - p

Ghanaian l other elements. ,,.-ttt

With the use of dithiapyrylmethane pro- I IG G

bismuth determinations in polymetal-Hz-x are made

ores, gold in electrolytes and industrial 5N1

waters of electroplating shops, tellurium in us-g and vi

sh ksoderzhaschih concentrates.

The formula of the invention is yes, alkyl, aryl, alkylaryl or halogen, and derivatives of dithiolarylmethane with formulas of noble metals.

515747

where RI and Co each denote an atom of hydrogen-complexing ability