Thiosulfuric acid derivant preparation

A compound, CH2 technology, applied in the direction of organic chemistry, etc., can solve problems such as no examples given

Active Publication Date: 2005-11-23
LANXESS DEUTDCHLAND GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: firstly the diol and thiosulfate must be dehydrated by distillation before the reaction starts; secondly a large amount of organic solvent (diol and precipitant) must be handled
Nor is any example given for the synthesis of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a nitrogen-purged, 2-liter four-neck stirred flask with built-in thermometer, reflux condenser with bubble gauge, and pH electrode, 300 g of demineralized water and 136.5 g (0.55 mol) of sulfur pentahydrate were charged with stirring sodium sulfate. After the thiosulfate was dissolved, 38.8 g (0.25 mol) of 1,6-dichlorohexane was added. The weakly acidic mixture was adjusted to pH 7.2 with a few drops of 2.5% sodium hydroxide solution. Once again the reaction vessel was briefly flushed with nitrogen, the mixture was then boiled under reflux for 9 hours, and 2.5% sodium hydroxide solution was added by means of a metering pump, so that during this time the pH of the reaction mixture was maintained at 7.2±0.1 (pH electrode) . After each reaction for 6 and 8 hours, the bubble gauge was briefly removed from the reflux condenser. In each case about 5 ml of demineralized water was sprayed into the reflux condenser from the top of the reflux condenser through the wash bott...

Embodiment 2 to 5

[0050] The procedure of Example 1 was repeated except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9, respectively. Before starting the specific reaction, the pH of the weakly acidic mixture was adjusted to 5, 6, 8 and 9 (measured with a pH electrode) with 2.5% sodium hydroxide solution.

Embodiment 2     Embodiment 3

[0051] Example 2 Example 3 Example 4 Example 5

[0052] pH value during reaction 5.0±0.1 6.0±0.1 8.0±0.1 9.0±0.1

[0053] residual 1,6-dichloro

[0054] Hexane content (ppm) <10 <10 <10 about 11

[0055] 1,6-Dichlorohexane

[0056] The conversion rate (%) >99.9 >99.9 >99.9 >99.9

[0057] In all examples (Examples 2 to 5), the resulting reaction mixtures were clear and homogeneous.

[0058] In order to determine the net yield of Examples 2 and 5, they were all repeated once. However, samples for GC analysis were not taken from specific reaction mixtures. Repeat Example 2, the net yield of (two) sodium salt (di) hydrate of hexamethylene 1,6-dithiosulfuric acid is about 91.4% 2) ; Repeat Example 5, the net yield is about 90.6% 2) .

[0059] 2) The syntheses of Examples 2 and 5 were carried out again like Example 1 by reacting the reaction solution obtained in each case with an aqueous NaBEC solution so as to obtain a net yield. In this step, according to...

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PUM

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Abstract

The invention relates to a novel process for preparing salts of S-alkyl esters of thiosulphuric acid by reacting organic dihalides with thiosulphates in water.

Description

technical field [0001] The present invention relates to a process for the preparation of salts of S-alkyl esters of thiosulfuric acid. Background technique [0002] The principle of preparation of salts of S-alkyl esters of thiosulfuric acid (Bunte salts) is known (ref: e.g. B. Milligan and J.M. Swan in Rev. Pure and Applied Chemistry 12, 1962, pp. 72 to 94, and H. Distler in Angew. Chem. 79, 1967, pp. 520-529). [0003] According to B. Milligan et al., Bunte's salt can generally be prepared by reacting an alkyl halide and sodium thiosulfate in a boiling solution of 50% aqueous ethanol (page 74, right column, third paragraph). Water is used as the sole solvent only in the case of water-soluble alkyl halides. [0004] EP-A 70 143 describes the use of a 1:1 mixture of water and ethanol as solvent for the preparation of the sodium salt hydrate of hexamethylene 1,6-dithiosulfuric acid. However, the disclosed solvents of this invention are ethylene glycol and diethylene glycol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/02C07C381/00
CPCC07C381/02
Inventor H·布丁
Owner LANXESS DEUTDCHLAND GMBH
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