Method for detecting content of pyridine-3-sulfonyl chloride

Abstract

The invention relates to a method for detecting the content of pyridine-3-sulfonyl chloride, which comprises the following steps: S1, derivatization: by taking acetonitrile as a solvent, adding excessive aniline and a pyridine-3-sulfonyl chloride sample to be detected, stirring to react, and diluting with an acetonitrile aqueous solution to obtain a test solution; s2, liquid chromatography detection: taking octadecylsilane chemically bonded silica as a filler of a chromatographic column, adopting an ultraviolet detector, taking a 0.2% tetrabutyl ammonium hydroxide phosphate buffer solution as a mobile phase A and taking acetonitrile as a mobile phase B, mixing the mobile phase A and the mobile phase B according to a ratio, carrying out isocratic elution on the test sample solution, controlling the detection wavelength to be 230nm, the flow velocity to be 0.5-1.5 mL / min and the sample injection volume to be 5-100mu L, and carrying out gradient elution on the test sample solution according to the detection wavelength of 230nm, the flow velocity to be 0.5-1.5 mL / min and the sample injection volume to be 5-100mu L; the column temperature is 25-40 DEG C; when being used for detecting the content of pyridine-3-sulfonyl chloride, the method provided by the invention has the advantages of good accuracy and repeatability, strong specificity, high accuracy and simplicity in operation.

Description

technical field [0001] The invention belongs to the field of organic matter analysis and detection, in particular to a method for detecting the content of pyridine-3-sulfonyl chloride. Background technique [0002] Pyridine-3-sulfonyl chloride is a commonly used pharmaceutical intermediate. It is a colorless and transparent liquid, which is extremely unstable in the presence of water, and is easily hydrolyzed to generate pyridine-3-sulfonic acid and hydrochloric acid, making it inactive. It can be used for the synthesis of pyrimidine derivatives and is an intermediate for the synthesis of vonoprazan fumarate. [0003] At present, the main determination method for the content of pyridine-3-sulfonyl chloride is titration method (the method for determining the content of pyridine-3-sulfonyl chloride. Invention patent application specification CN201510220469.0). The amount of free acid to calculate its content. The disadvantages of this titration method are: 1) The specificity...

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Problems solved by technology

The disadvantages of this titration method are: 1) The specificity is poor. When pyridine-3-sulfonyl chloride contains other impurities that can dissociate chloride ions, it will interfere with the titration results

2) During the titration process of free acid, a mixture of ice and water should be added to keep the solution of the test product at 0°C. This process is easily affected by the ambient temperature, and adding water to the test product cannot guarantee that the test product will not undergo hydrolysis reaction

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