Method for determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation

A technology of dichloroacetophenone and gas chromatography, which is applied in the directions of material separation, measurement device, analysis material, etc., can solve the problems such as separation and measurement that have not been reported in the literature.
CN108445121AActive Publication Date: 2018-08-24常州市盛辉药业有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
常州市盛辉药业有限公司
Publication Date
2018-08-24

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Abstract

The invention discloses a method for determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation. According to the method, an HP-5 weak-polarity capillary column is adopted and has the specification of 30m*0.32mm*0.5mu m; carrier gas is nitrogen gas and the flow speed of the carrier gas is 1.0mL / min; a hydrogen flame detector is adopted; the temperature of a sample feeding opening of a gas chromatograph is 200 to 280 DEG C, the temperature of a column box is 130 to 180 DEG C and the temperature of the detector is 250 to 300 DEG C; constant-temperature separation is carried out and the sample feeding amount is 2mu L; finally, separation of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone is realized; chromatographic conditions are provided for quantitative detection of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone.
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Description

technical field

[0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for separating and measuring 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by gas chromatography. Background technique

[0002] 2,4-Dichloroacetophenone is a light yellow solid, an important fine chemical intermediate, widely used in medicine, pesticide and other fields. It is the first clinically available oral broad-spectrum antifungal drug ketoconazole [cis-[2-(2,4-dichloro)-2-(1H-imidazolyl-1-methanol) Base)-1,3-dioxolane-4-]methyl p-toluenesulfonate (active ester) intermediate is an important raw material.

[0003] Because inevitably can produce a certain amount of 2,6-dichloroacetophenone (isomers) in the synthetic process of 2,4-dichloroacetophenone, the 2,6-dichloroacetophenone The purity of 2,4-dichloroacetophenone is affected, thereby affecting the synthetic effect of ketoconazole.

[0004] The separation and identifi...

Claims

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