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A method for the separation and determination of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by gas chromatography

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 of separation and measurement that have not been reported in literature and the like

Active Publication Date: 2021-06-25
常州市盛辉药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no literature report on the separation and determination of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers

Method used

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  • A method for the separation and determination of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by gas chromatography
  • A method for the separation and determination of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by gas chromatography
  • A method for the separation and determination of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by gas chromatography

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Embodiment 1

[0027] 1. Instrument

[0028] Gas chromatograph: Shimadzu, GC-2014AT, hydrogen flame detector.

[0029] Chromatographic column: HP-5 (30m×0.32mm×0.5μm).

[0030] 2. Chromatographic conditions

[0031] Carrier gas: nitrogen

[0032] Flow rate: 1.0 mL / min.

[0033] Detector: hydrogen flame detector.

[0034] Injector temperature: 250°C.

[0035] Detector temperature: 280°C.

[0036] Column temperature: 170°C.

[0037] Injection volume: 2 μL.

[0038] Using constant temperature separation.

[0039] 3. Experimental steps

[0040] Weigh 5g of 2,4-dichloroacetophenone and 5g of 2,6-dichloroacetophenone into a 100mL volumetric flask, dissolve and dilute to the mark with ethanol solution, and shake well to obtain a sample solution.

[0041] Take 2 μL of the above solution, analyze according to the above chromatographic conditions, and record the chromatogram, the results are as follows: figure 1 shown.

[0042] figure 1 The chromatographic peak with a retention value of 4...

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Abstract

The invention discloses a method for separating and measuring 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by gas chromatography, using an HP-5 weakly polar capillary column with a specification of 30m× 0.32mm×0.5μm, the carrier gas is nitrogen, the carrier gas flow rate is 1.0mL / min, a hydrogen flame detector is used, the gas chromatograph inlet temperature is 200~280℃, the column oven temperature is 130~180℃, and the detector temperature is 250 ~300°C, constant temperature separation, injection volume is 2 μL, and finally achieved the separation of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone into 2,4-dichloroacetophenone and 2 , providing chromatographic conditions for the quantitative detection of 6-dichloroacetophenone.

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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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/68G01N30/06
CPCG01N30/06G01N30/68
Inventor 陈舟
Owner 常州市盛辉药业有限公司
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