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Amphiprotic compound containing sulphur, its preparing method and usage

A compound, amphoteric technology, applied in the field of amphoteric sulfur-containing compounds and their preparation, can solve the problems of undiscovered amphoteric sulfur-containing compounds, loss of organic reagents, environment, pollution, etc. Effect

Inactive Publication Date: 2003-10-01
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in B.V. Depamphilis et al. Synthetic analogs of the active sites of iron-sulfur proteins.VI. Spectral and redox characteristics of the tetranuclear clusters [Fe 4 S 4 (SR) 4 ] 2- (J.Am.Chem.Soc.1974,26,4159-4161) discloses a kind of sulfur-containing compound 4-trimethylammonium thiophenol hexafluorophosphate and its synthetic method, 4-trimethylammonium thiophenol Hexafluorophosphate is an amphoteric sulfur-containing compound that can be used in the synthesis of multinuclear polymers and clusters, but it is insoluble in water. In fact, most sulfur-containing compounds can only be dissolved in organic reagents, which will inevitably cause a large amount of Loss of organic reagents and environmental pollution
After searching the literature, no ideal amphoteric sulfur-containing compounds have been found so far

Method used

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  • Amphiprotic compound containing sulphur, its preparing method and usage
  • Amphiprotic compound containing sulphur, its preparing method and usage
  • Amphiprotic compound containing sulphur, its preparing method and usage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Add 1.00 molar parts of dichlorodisulfide dropwise to 1.10 molar parts of N, N dimethylaniline in a benzene solution, stir for 2 hours to obtain a yellow sticky substance; then add 2.0 molar parts of methyl iodide acetone Solution; After stirring for 48 hours, a white solid was obtained by filtration, and the reaction condition was 0°C.

[0020] Dissolve the product obtained in the above steps in water, add 8.0 molar parts of hydrochloric acid and 5.0 molar parts of zinc powder, stir for 5.0 h, filter off excess zinc powder, add 1.8 molar parts of ammonium hexafluorophosphate to the solution, and stir for 1.0 hour, The white solid 4-trimethylammonium thiophenol hexafluorophosphate was obtained by filtration, and the reaction condition was 40±2°C.

[0021] Dissolve 1.0 molar part of 4-trimethylammonium thiophenol hexafluorophosphate in 150 ml of acetonitrile, add 1.0 molar part of triethylamine dropwise, filter and wash with ether to obtain a white powdery sol...

Embodiment 2

[0045] Example 2: Dissolve 1.0 molar parts of 4-trimethylammonium thiophenol hexafluorophosphate in 150 ml of acetonitrile, add 1.25 molar parts of triethylamine dropwise, filter and wash with ether to obtain a white powdery solid with a purity of 82.5%. . The reaction condition is 10±1°C, and the reaction time is 2.5h.

[0046] Dissolve the above-mentioned white powdery solid in a mixed solvent of 500ml of water and methanol (volume ratio 1:5) at room temperature, add diethyl ether dropwise, and precipitate colorless needle-like crystals, and dry them in vacuum at 40°C to obtain the product of the present invention. The rate is 77%.

Embodiment 3

[0047] Example 3: Dissolve 1.0 molar parts of 4-trimethylammonium thiophenol hexafluorophosphate in 150 ml of acetonitrile, add 1.5 molar parts of triethylamine dropwise, filter and wash with ether to obtain a white powdery solid with a purity of 89% . The reaction condition is 10±1°C, and the reaction time is 3h.

[0048] Dissolve the above-mentioned white powdery solid in a mixed solvent of 500ml of water and methanol (volume ratio 1:5) at room temperature, add diethyl ether dropwise, and precipitate colorless needle-like crystals, and dry them in vacuum at 40°C to obtain the product of the present invention. The rate is 74%.

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Abstract

A S-contained amphoteric compound containing the cation of quaternary ammonium salt and the anion of benzenethiol is prepared through dissolving 4-trimethylamine benzenethiol hexafluorophosphate in organic solvent, dropping triethylamine to generate white deposit, reaction filtering, and washing to obtain white powder used as S-contained ligand.

Description

technical field [0001] The invention relates to an amphoteric sulfur-containing compound and a preparation method thereof, and also relates to the use of the amphoteric sulfur-containing compound in the synthesis of metal complexes, clusters and polymers. Background technique [0002] Amphoteric sulfur-containing compounds react with metal ions to form a series of very interesting multinuclear polymers and clusters, and studies have shown that such clusters have certain application prospects in biopharmaceuticals. For example: in Preparation of complexes of the 3-trimethylammonio-1-propanathiolato ligand[M{S(CH 2 ) 3 NMe 3} 2 ](PF 6 ) 2 , M=Zn, Cd, Hg. CrystalStructures of monomeric and polymeric forms of the mercury complex (Inorg. Chim. Acta 1991, 184, 167-175) reported that mercury (II) compounds react with amphoteric sulfur-containing compounds to form Triphenylphosphine gold(I) complexes of sterically demanding and nondemanding arenethiols....

Claims

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Application Information

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IPC IPC(8): C07C319/14C07C323/35
Inventor 朗建平陈金香徐庆锋
Owner SUZHOU UNIV
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