Detection method of 2-(thiophene-2-yl)ethyl p-toluenesulfonate and isomers thereof

Abstract

The invention belongs to the field of medicines, and particularly relates to a detection method and application of 2-(thiophene-2-yl)ethyl p-toluenesulfonate and isomers thereof. The detection methodcomprises the steps of preparing a test solution, a reference solution and a system applicability solution; and carrying out high performance liquid chromatography detection on the test solution, thereference solution and the system suitability solution, wherein the detection conditions are as follows: the chromatographic column comprises a chiral chromatographic column taking silica gel coated with cellulose-tri(4-methyl benzoate) as a filling agent, the mobile phase comprises a mixed solution of n-hexane and absolute ethyl alcohol, and the flow velocity of the mobile phase is 0.7mL / min-0. 9mL / min, the detection wavelength ranges from 220nm to 227nm, the column temperature of the chromatographic column is 25-40 DEG C. The detection method is good in sensitivity, high in accuracy, good inreproducibility, convenient to operate and good in durability, the quality of 2-(thiophene-2-yl)ethyl p-toluenesulfonate can be effectively controlled, and the detection method has important significance in controlling the quality of clopidogrel hydrogen sulfate from the source.

Description

technical field [0001] The invention belongs to the field of medicines, in particular to a detection method for 2-(thiophen-2-yl)ethyl p-toluenesulfonate and its isomers. Background technique [0002] 2-(thiophen-2-yl) ethyl p-toluenesulfonate is the key starting material for the synthesis of clopidogrel hydrogen sulfate, and in the process of synthesizing 2-(thiophen-2-yl) ethyl p-toluenesulfonate Often accompanied by the generation of by-product 2-(thiophen-3-yl)ethyl p-toluenesulfonate, the two are positional isomers on the thiophene ring, and positional isomer impurities are similar in nature due to the main components. The method is usually difficult to separate, and positional isomer impurities are often transferred to intermediates and even raw materials because they contain the same active group as the main component, directly affecting the purity and quality of raw materials. There is no detection method for 2-(thiophen-2-yl) ethyl p-toluenesulfonate and its isomer...

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Problems solved by technology

[0002] 2-(thiophen-2-yl) ethyl p-toluenesulfonate is the key starting material for the synthesis of clopidogrel hydrogen sulfate, and in the process of synthesizing 2-(thiophen-2-yl) ethyl p-toluenesulfonate Often accompanied by the generation of by-product 2-(thiophen-3-yl)ethyl p-toluenesulfonate, the two are positional isomers on the thiophene ring, and positional isomer impurities are similar in nature due to the main components. The method is usually difficult to separate, and positional isomer impurities are often transferred to intermediates and even raw materials because they contain the same active group as the main component, directly affecting the purity and quality of raw materials

There is no detection method for 2-(thiophen-2-yl) ethyl p-toluenesulfonate and its isomers at present, so a kind of 2-(thiophen-2-yl) ethyl p-toluenesulfonate is established The detection method of its isomer 2-(thiophen-3-yl)ethyl p-toluenesulfonate is very important to control the quality of clopidogrel bisulfate from the source

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