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Method for determining content of pyridine-3-sulfonyl chloride

A technology of sulfonyl chloride and pyridine, applied in the field of chemical analysis, can solve problems to be improved, etc., and achieve the effects of short time consumption, accurate results, good specificity and accuracy

Inactive Publication Date: 2016-12-07
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Therefore, the current method for measuring pyridine-3-sulfonyl chloride content still needs to be improved

Method used

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  • Method for determining content of pyridine-3-sulfonyl chloride
  • Method for determining content of pyridine-3-sulfonyl chloride
  • Method for determining content of pyridine-3-sulfonyl chloride

Examples

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preparation example Construction

[0030] The preparation process of pyridine-3-sulfonyl chloride is as follows:

[0031]

Embodiment 1

[0033] Weigh about 0.6g of this product, weigh it accurately, place it in a 50ml volumetric flask, add acetone to dissolve and dilute to the mark, shake well, and use it as the sample stock solution. Precisely measure 10ml of sample stock solution, put it in a 100ml beaker, add 2ml of 1.5mol / L sodium hydroxide solution, add 50ml of water to dilute, decompose under magnetic stirring for 5-10min, add dropwise 5ml of 10% nitric acid solution, and use 0.1mol / L silver nitrate titration solution is titrated to the end point by potentiometric titration, and the titration result is corrected with a blank test to calculate the total chlorine content in the sample solution; in addition, 10ml of the sample stock solution is accurately measured, put in a 100ml beaker, and add ice-water mixture to 80ml (to keep the test solution to be tested at 0 degrees Celsius until the titration ends), decompose it under magnetic stirring for 5min, use 0.1mol / L silver nitrate titration solution to titra...

Embodiment 2

[0051] Weigh about 0.6 g of the sample used in Example 1, weigh it accurately, place it in a 50 ml volumetric flask, add acetonitrile to dissolve and dilute to the mark, shake well, and use it as a sample stock solution. Precisely measure 10ml of sample stock solution, put it in a 100ml beaker, add 5ml of 2.5mol / L sodium hydroxide solution, add 50ml of water to dilute, decompose under magnetic stirring for 5-10min, add dropwise 10ml of 10% nitric acid solution, and use 0.1mol / L silver nitrate titration solution is titrated to the end point by potentiometric titration, and the titration result is corrected with a blank test to calculate the total chlorine content in the sample solution; in addition, 10ml of the sample stock solution is accurately measured, put in a 100ml beaker, and add ice-water mixture to 80ml, under magnetic stirring, titrate to the end point with 0.1mol / L silver nitrate titration solution by potentiometric titration, and the titration result is corrected wi...

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Abstract

The invention discloses a method for determining content of pyridine-3-sulfonyl chloride. The method comprises the following steps: 1) weighing a sample, adding an organic solvent for dissolving the sample to prepare a sample stock solution; 2) weighing the sample stock solution, adding an alkaline solution, adding water for dilution, dropping a nitric acid solution, using a first titration solution for potentiometric titration, calculating total chlorine amount in the sample; 3) weighing the sample stock solution, adding water for dilution, dropping the nitric acid solution, using a second titration solution for potentiometric titration, calculating free acid amount in the sample; and 4) calculating content of pyridine-3-sulfonyl chloride in the sample. The method has the advantages of strong specialization, high precision, strong accuracy, and simple and rapid operation, and can realize the accurate detection of the content of pyridine-3-sulfonyl chloride.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for determining the content of pyridine-3-sulfonyl chloride. Background technique [0002] Pyridine-3-sulfonyl chloride (PYRIDINE-3-SULFONYL CHLORIDE, the compound shown in formula 1) is a commonly used pharmaceutical intermediate, which is a colorless transparent liquid, extremely unstable in contact with water, and easily hydrolyzed to generate pyridine-3-sulfonic acid and hydrochloric acid to make it inactive. The existing detection methods are mainly to add derivatization reagent to pyridine-3-sulfonyl chloride and then detect by gas chromatography, or use gas chromatography to directly inject samples, or directly detect by nuclear magnetic resonance spectroscopy. The disadvantages of gas chromatography detection are mainly: 1) the degree of derivatization is not easy to control; 2) pyridine-3-sulfonic acid can also react with derivatization reagents, and like pyrid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 徐先英钱丽娜
Owner WATERSTONE PHARMA WUHAN
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