SU1634668A1 - N-(2,3-tetramethylene-4-thenoyl)-n-(4-tolylsulfonyl) hydrazine for extraction photometric determination of osmium - Google Patents

Description

(21) 4606530/04

(22) 11/15/88

(46) 03/15/91. Bul Number 10

(71) Perm State University. AM Gorky and the Institute of Organic Chemistry of the Ural Branch of the USSR Academy of Sciences

(72) N.Ye. Vorobeva, P.T. Pavlov, Yu.V.Shklyev and V.P. Zhivopistsev

(53) 547.732 (088.8)

(56) USSR Author's Certificate No. 1516974, cl. G 01 N31 / 22, 1987.

(54) M- (2,3-TETRAMETHYLENE-4-TENOIL) - -N- (4-TOLYLSULPHONE) HYDRAZINE FOR EXTRACTION-EDTOMETRIC DETERMINATION OF OSMY

(57) The invention relates to derivatives of heterocyclic substances, in particular N - (2,3-tetramethylene-4-tenoyl) -M- (4-tolylsulfonyl) hydrazine,

which possesses the properties of an extraction photometric reagent and can be used in analytical chemistry. The purpose of creating a new, more effective reagent of the specified kpassa. Synthesis is carried out by the reaction of hydrazide 2,3-tetramethylene-4-thiophenecarboxylic acid with p-toluenesulfonyl chloride in pyridine at room temperature. Output 86%, t „„ 171-172 ° С, gross f-la C16. This reagent increases the sensitivity of osmium detection, expands the range of hydrochloric acid concentrations in which complexing is observed, and contributes to the quantitative extraction of this element and the possibility of extracting osmium in a wide range of sulfuric acid concentrations. 1 tab.

se

(L

This invention relates to the chemistry of organic sulfur compounds, namely, to a new chemical compound N - (2, 3-tetramethylene-4-thenoyl) -N- - (4-topylsulfonyl) hydrazine of Formula (I):

sn (i)

H2SL / SOYNY802NO CH3

H c (sJ

which possesses the properties of an extraction photometric reagent and

can be used in analytical chemistry.

The aim of the invention is to identify a new reagent of formula (I), which makes it possible to increase the sensitivity of the determination of osmium, expand the range of hydrochloric acid concentrations, in which complex formation and copious quality extraction of this element is observed, as well as to achieve the possibility of extracting osmium in a wide range of concentrations of sulfuric acid. acid versus analogous in structure and purpose

with

Ј

ABOUT

oh

00

N -2-hydroxybenzoyl-K- (4-tolylsulfonyl) hydrazine (II).

Example 1. Synthesis of N - (2,3-tetramethylene-4-thenoyl) -M- (4-tolylsulfonyl) hydrazine: 1.0 g (0.005 mol) of hydrazine 2, 3-tetramethylene-4-thiophen- The carboxylic acids are dissolved in 15.0 cm of pyridine, 0.95 g (0.005 mol) of p-toluenesulfonyl chloride is added and left at room temperature until next day. Dilute the reaction mass with water, and triturate the resulting resin with a glass rod before crystallization. The precipitate is filtered off, washed with water and dried at 40-50 ° C. Yield 1.5 g (86%). From toluene needles from 171-172 ° C. Rf 0.54 (Silufol) UB-254, benzene: ether-3: 2. The white substance is soluble in DMF, DMSO, ethanol, chloroform, acetone, dioxane, aqueous alkalis. It is difficult soluble in benzene, toluene, carbon tetrachloride, hexane.

Found,%: C 54.68; H 5.09; N 7.85; B 18.24.

C, 6H, eN203Sz.

Calculated,%: C 54.84; H 5.17; N 7.99; S 18.30. (

IR spectrum, vaz.maslo N ddChKS, cm: 3210 NH (CO) NH (S02) J, ZPO (C – H-thiophene ring), 1635 (CO), 1335, 1170 (50), 820, 840 (4-CgH -).

PMR spectrum, 8% solution in DMSO d ,, ppm: 10.33 (1H, NHS02)} 9.80 (1H, NHCO); 7.66, 7.25 (4H; 4-C6Hf); 2.43 n (CH2) g-2,3-shade-, 28 (3N, CH3); 1.55 f 4H (CH2) g

PRI mme R 2. Definition osmi (VI) N - (2,3-tetramethylene-4 thienyl) - -N- (4-tolylsulfonyl) hydrazine.

A standard alkaline solution containing (VI) is added to the separatory funnel, the alcohol solution of the reagent is added, the acidity of the aqueous phase in a volume of 20 ml, equal to 2 M for sulfuric acid is added, and the contents of the funnel are agitated for 10 minutes with 10 ml

 mcg osmi 0.5 ml 1) M

5 0 5

0

five

0

five

100x and 50s0

chloroform. The organic phase is separated and the optical density of the extracts is measured on a KFK-2MP 1 2 cm photocolorimeter, J 540 nm relative to a pure solvent.

The definition of osmium by the proposed reagent does not interfere with alkaline and alkaline-earth elements, as well as 100-fold molar excesses (Cr (VI), Mo (VI); 500 - Cu (II); Fe (III); 100 - Ni (II), Pt ( IV), Au (III) 1 h (III); 50 - Co (II), Ag; 20 - Pd (II); 10-Rh (III) Ru (IV), Ru (VI); 2000 - multiple molar excess of chloride -, sulfate-, nitrate-, carbonate-ions; excess - telluride-ions of nid-ions.

The table shows the comparative characteristics of the determination of osmium by a known method using N -2-hydroxybenzoyl-M- (4-tolylsulfonyl) hydrazine and the reagent (I) proposed.

Thus, the new reagent I for the extraction of photometric determination of osmium has a higher sensitivity than the known reagent II, allows to significantly expand the concentration range of hydrochloric acid, in which quantitative extraction of osmium is observed, and also allows the quantitative extraction of osmium from sulfuric acid solutions.

Claims (1)

Invention Formula N - (2,3-Tetramethylene-4-tenoyl) -M - (4-tolylsulfonyl) hydrazine of the formula CH7 H2CxiY-n-CONHNHS02H cc sJ for the extraction-photometric determination of osmi. 1634668 Known reagent Indicators I wg  , 1-15 7, 15-Ю3 pH 3-1 M HC1 pH 3-4 M H2SO580 98-99 Co (50), Fe (100), Ni Cu (500), Ag (200), Au (5), Pd (10), Pt (IOO), Rh (lC), Ir (50), Ru (100) The result was obtained for comparison with the proposed reagent. The proposed reagent 0.5-15 8.3-U3 pH 5-6 M HC1 pH 3-8 M Ng504 540 t 98-99 100), Co (10), Pe (500), N1 (100), Cu (500), Ag (50), Au (100), Pd (20), Pt (IOO), Rh (IO), Ir ( 100), Ru (10.0)