2-(2-hydroxyphebyl)-2-(r'-phenyl)-1,3,4-thiadiazolines-2 used as analytical reagents

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to preparing analytical reagents eliciting selectivity and high sensitivity with respect to transient metal cations. Method involves interaction of 2-hydroxythiobenzoyl hydrazone with aromatic aldehydes that results to synthesis of 2-(2'-hydroxyphenyl)-5-(R'-phenyl)-1,3,4-thiadiazolines-2 that have been tested as analytical reagents with metal cation salts of s-, p- and d-elements. Obtained results of investigations have been applied for analysis of medicinal agents containing transient metal cations. Invention provides expanding assortment of analytical reagents used for detection of metal cations of s-, p- and d-elements that can be used in analytical, pharmaceutical and chemical-toxicological practice.

EFFECT: valuable properties of reagents.

1 cl, 2 tbl, 3 ex

 

The invention relates to the search for new analytical reagents, namely the synthesis of the compounds used for the detection of metal cations s-, p - and d-elements.

With the aim of obtaining analytical reagents possessing selectivity and high sensitivity with respect to cations of transition metals, the interaction of 2-hydroxydibenzofuran with aromatic aldehydes were synthesized 2-(2’-hydroxyphenyl)-5-(R’-phenyl)-1,3,4-thiadiazoline-2, which were tested as analytical reagents with metal salts of s-, p - and d-elements.

Experimental data have shown that 2,5-bis-(2-hydroxyphenyl)-1,3,4-thiadiazoline-2 (compound I) with cations of Nickel, aluminum, magnesium and copper form a precipitation of yellow and brown color with a characteristic microcristallina:

2-(2-hydroxyphenyl)-5-(2-chlorophenyl)-1,3,4-thiadiazoline-2 (compound II)

with cations of iron sludge forms lilac, partially soluble in diluted chloroethanol acid;

- with cations of magnesium - yellow precipitate with a characteristic microcristallina;

2-(2-hydroxyphenyl)-5-(4-nitrophenyl)-1,3,4-thiadiazole-2 (compound III) forms with cations of Nickel precipitate red;

2-(2-hydroxyphenyl)-5-(4-methoxyphenyl)-1,3,4-thiadiazoline-2 (compound IV) forms:

with the cations of zinc bright yellow gelatinous, ocado is, soluble in diluted chloroethanol acid;

with the cantons of iron (II) - light grey precipitate;

with cobalt cations - light-brown precipitate;

with the cantons copper - light green precipitate;

- with cations of lead - yellow-green precipitate;

- with cations bismuth - lemon-yellow crystals with a characteristic crystallography.

The obtained results were used for the qualitative analysis of medicinal products containing cations of bismuth (de-Nol, Tribunal in the form of bismuth subcitrate); vikair, usually in the form of bismuth nitrate basic), and magnesium (Panangin in the form of magnesium Asparaginate).

The experimental data showed a positive result:

for bismuth cations at the limiting dilution 1:10000, open a minimum of 2.92 µg;

for cations of magnesium at the limiting dilution 1:13000, openable to a minimum of 2.36 µg;

for cations of Nickel at the limiting dilution 1:17000, openable to a minimum of 1.75 µg.

Thus, 2-(2-hydroxyphenyl)-5-(R-phenyl)-1,3,4-thiadiazoline-2 showed the promise of using them as a highly sensitive analytical reagents for the detection of metal cations s-, p - and d-elements. This allows you to expand the list of analytical reagents used in analytical, pharmaceutical and chemical-Toxicological practice is E.

The way to obtain

Example 1. Dissolve 2,72 g disalicylidene in 10 ml of ethanol when slightly heated. To the resulting solution was added to 0.73 ml of salicylic aldehyde (d=1,67) in 5 ml of ethanol. After heating for 10 minutes the solution is cooled, filtered, washed and dried. Gain of 1.30 g (47,79%) of 2,5-bis-(2-hydroxyphenyl)-1,3,4-thiadiazoline-2 (compound I) in the form of light yellow needle crystals. A similar methodology was obtained compound (II-IV (table 1).

Example 2. Obtaining a complex of 2,5-bis-(2-hydroxyphenyl)-1,3,4-thiadiazoline-2 with magnesium cations. When adding 1 ml of 0.1 M solution of magnesium sulfate 4-5 drops of 0.02% alcohol solution of 2,5-bis-(2-hydroxyphenyl)-1,3,4-thiadiazoline-2 observing the turbidity of the solution and precipitation of a crystalline precipitate of magnesium bis-(2-hydroxybenzaldehyde-2-hydroxy-dibenzoylhydrazine) bright yellow color, with a characteristic microcrystallization as bundles of needles and yellow sockets. Complexes of other transition metal cations with 2-(2-hydroxyphenyl)-5-(R-phenyl)-thiadiazoline-2 was obtained by the same methodology (table 2).

Example 3. Analysis of metal cations contained in the medicines.

About 0.5 g of crushed tablets Panangin containing magnesium Asparaginate, dissolved in 5 ml of 30° ethanol and filtered off from accompanying substances.

When is the adding to 1 ml of the resulting filtrate to 5 drops of 0.002% alcohol solution of 2-(2-hydroxyphenyl)-5-(2-chlorophenyl)-1,3,4-thiadiazoline-2 is formed yellow precipitate of magnesium bis-(2-chlorobenzaldehyde-2-hydroxy-dibenzoylhydrazine).

Detection of bismuth cations were produced in tablets de-Nol and tribioli (containing bismuth subcitrate), as well as in tablets viceira and usually (containing bismuth nitrate basic) after pre-dilution mass of crushed tablets in diluted nitric acid by a similar method.

2-(2’-hydroxyphenyl)-5-(R’-phenyl)-1,3,4-thiadiazoline-2 formula

whereused as analytical reagents.



 

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