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Method for detecting purity of 2-chloropropionyl chloride

A technology for the purity and detection method of chloropropionyl chloride, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as unstable results, damage to testing instruments, and research on undetected methods, so as to avoid unstable measurement results and avoid corrosion Effect

Active Publication Date: 2019-11-12
HARVEST PHARMA HUNAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the acid chloride group in 2-chloropropionyl chloride can be hydrolyzed, the result obtained by direct detection is unstable, and the acid chloride group has very strong oxidation and corrosion, which is easy to cause damage to the test instrument
Patent CN109060978A provides a gas-phase detection method for the content of acryloyl chloride, which utilizes the derivatization treatment of acryloyl chloride and aniline to form amides, and then detects acryloyl chloride by internal standard method detection, but aniline is a highly toxic substance with a strong odor. And the patent did not conduct detailed research on the detection method

Method used

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  • Method for detecting purity of 2-chloropropionyl chloride
  • Method for detecting purity of 2-chloropropionyl chloride
  • Method for detecting purity of 2-chloropropionyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Chromatographic conditions

[0031] Gas chromatograph: Agilent 7890B gas chromatograph;

[0032] Gas chromatography column: dimethylpolysiloxane (30m*0.53mm, 3μm);

[0033] Injection volume: 1μl;

[0034] Detector temperature: 250°C;

[0035] Front inlet temperature: 250°C;

[0036] Detector: FID;

[0037] Split ratio: 10:1;

[0038] Flow rate: 3ml / min;

[0039] Heating program: the initial temperature is 40°C, keep for 6min, then rise to 250°C at 15°C / min, and keep for 5min.

[0040] (2) Sample preparation

[0041] Sample solution preparation: Slowly add 1g of chloropropionyl chloride dropwise to a 10ml volumetric flask containing 8ml of ethanol, wait to cool to room temperature, add ethanol to the mark, and shake well to obtain.

[0042] (3) Detection method

[0043] The autosampler extracts 1ul and injects it into the gas chromatograph, the chromatogram is as follows figure 1 shown.

[0044] (4) calculation

[0045] Calculated by area normalization me...

Embodiment 2

[0058] (1) Chromatographic conditions

[0059] Gas chromatograph: Agilent 7890B gas chromatograph;

[0060] Gas chromatography column: dimethylpolysiloxane (30m*0.53mm, 3μm);

[0061] Injection volume: 1μl;

[0062] Detector temperature: 250°C;

[0063] Front inlet temperature: 250°C;

[0064] Detector: FID;

[0065] Split ratio: 10:1;

[0066] Flow rate: 3ml / min;

[0067] Heating program: the initial temperature is 80°C, keep for 6min, then rise to 250°C at 10°C / min, and keep for 5min.

[0068] (2) Sample preparation

[0069] Sample solution preparation: Slowly add 1g of chloropropionyl chloride dropwise to a 10ml volumetric flask containing 8ml of ethanol, wait to cool to room temperature, add ethanol to the mark, and shake well to obtain.

[0070] (3) Detection method

[0071] The autosampler draws 1ul and injects it into the gas chromatograph.

[0072] (4) calculation

[0073] Calculated by area normalization method.

[0074] (5) Experimental results

[0075] ...

Embodiment 3

[0081] (1) Chromatographic conditions

[0082] Gas chromatograph: Agilent 7890B gas chromatograph;

[0083] Gas chromatography column: dimethylpolysiloxane (30m*0.53mm, 3μm);

[0084] Injection volume: 1μl;

[0085] Detector temperature: 250°C;

[0086] Front inlet temperature: 250°C;

[0087] Detector: FID;

[0088] Split ratio: 20:1;

[0089] Flow rate: 3ml / min;

[0090] Heating program: the initial temperature is 40°C, keep for 6min, then rise to 250°C at 15°C / min, and keep for 5min.

[0091] (2) Sample preparation

[0092] Sample solution preparation: Slowly add 1g of chloropropionyl chloride dropwise to a 10ml volumetric flask containing 8ml of ethanol, wait to cool to room temperature, add ethanol to the mark, and shake well to obtain.

[0093] (3) Detection method

[0094] The autosampler draws 1ul and injects it into the gas chromatograph.

[0095] (4) calculation

[0096] Calculated by area normalization method.

[0097] (5) Experimental results

[0098] ...

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Abstract

The invention discloses a method for detecting purity of 2-chloropropionyl chloride. The derivatization by utilizing the property that acyl chloride is easily reacted with an alcohol to form an estersubstance avoids the corrosion and unstable determination result caused by direct determination of 2-chloropropionyl chloride, and the purity of 2-chloropropionyl chloride is calculated by an area normalization method through gas chromatography. The detecting method can effectively separate the main component peak and impurity peaks of 2-chloropropionyl chloride to greatly improve the detection sensitivity of 2-chloropropionyl chloride, thereby detecting the purity of 2-chloropropionyl chloride simply, quickly and stably. The detecting method has the advantages of simple operation, high accuracy, high sensitivity and precision, good stability and good reproducibility.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a detection method for the purity of 2-chloropropionyl chloride. Background technique [0002] The English name of 2-chloropropionyl chloride is 2-Chloropropionyl chloride, the chemical name is 2-chloropropionyl chloride, the molecular formula is C3H4Cl2O, the molecular weight is 126.97, and its chemical structure is as follows: [0003] [0004] 2-chloropropionyl chloride is an important starting material for ibuprofen synthesis, and ibuprofen (Ibuprofen) is an antipyretic and analgesic non-steroidal anti-inflammatory drug, and the purity of 2-chloropropionyl chloride directly affects ibuprofen synthetic yield. Since the acyl chloride group in 2-chloropropionyl chloride can be hydrolyzed, the result obtained by direct detection is unstable, and the acyl chloride group has very strong oxidation and corrosion, which is easy to cause damage to the testing instrument. Pat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 袁金桥邹浩秦敏张瑜吴桐
Owner HARVEST PHARMA HUNAN CO LTD
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