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A method for effectively detecting the purity of 2-chloropropionyl chloride

A technology for the purity and detection method of chloropropionyl chloride, which is applied to measurement 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: 2022-06-10
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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  • A method for effectively detecting the purity of 2-chloropropionyl chloride
  • A method for effectively detecting the purity of 2-chloropropionyl chloride
  • A method for effectively detecting the 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: 1 μl;

[0034] Detector temperature: 250℃;

[0035] Front inlet temperature: 250℃;

[0036] detector: FID;

[0037] Split ratio: 10:1;

[0038] Flow rate: 3ml / min;

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

[0040] (2) Sample preparation

[0041] Preparation of sample solution: Slowly add 1g of chloropropionyl chloride dropwise to a 10ml volumetric flask containing 8ml of ethanol, let it cool to room temperature, add ethanol to the volume to the mark, and shake well.

[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] Calcula...

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: 1 μl;

[0062] Detector temperature: 250℃;

[0063] Front inlet temperature: 250℃;

[0064] detector: FID;

[0065] Split ratio: 10:1;

[0066] Flow rate: 3ml / min;

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

[0068] (2) Sample preparation

[0069] Preparation of sample solution: Slowly add 1g of chloropropionyl chloride dropwise to a 10ml volumetric flask containing 8ml of ethanol, let it cool to room temperature, add ethanol to the volume to the mark, and shake well.

[0070] (3) Detection method

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

[0072] (4) Calculation

[0073] Calculated by the area normalization method.

[0074] (5...

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: 1 μl;

[0085] Detector temperature: 250℃;

[0086] Front inlet temperature: 250℃;

[0087] detector: FID;

[0088] Split ratio: 20:1;

[0089] Flow rate: 3ml / min;

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

[0091] (2) Sample preparation

[0092] Preparation of sample solution: Slowly add 1g of chloropropionyl chloride dropwise to a 10ml volumetric flask containing 8ml of ethanol, let it cool to room temperature, add ethanol to the volume to the mark, and shake well.

[0093] (3) Detection method

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

[0095] (4) Calculation

[0096] Calculated by the area normalization method.

[0097] (5...

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Abstract

The invention discloses a detection method for the purity of 2-chloropropionyl chloride, which utilizes the property that the acid chloride is easy to react with alcohols to form esters for derivatization treatment, avoiding the corrosion caused by the direct measurement of 2-chloropropionyl chloride and the inaccurate measurement results. Stable, then by gas chromatographic detection, the final area normalization method calculates 2-chloropropionyl chloride purity. The detection method can effectively separate the main component peak and the impurity peak of 2-chloropropionyl chloride, which greatly improves the detection sensitivity of 2-chloropropionyl chloride, so that the purity of 2-chloropropionyl chloride can be detected simply, quickly and stably. The detection method is simple in operation, high in accuracy, high in sensitivity and precision, good in stability and good in reproducibility.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting the purity of 2-chloropropionyl chloride. Background technique [0002] 2-Chloropropionyl chloride English name 2-Chloropropionyl chloride, chemical name 2-chloropropionyl chloride, molecular formula is C3H4Cl2O, molecular weight is 126.97, its chemical structure is as follows: [0003] [0004] 2-Chloropropionyl chloride is an important starting material for the synthesis of ibuprofen. Ibuprofen (Ibuprofen) is an antipyretic and analgesic non-steroidal anti-inflammatory drug, and the purity of 2-chloropropionyl chloride directly affects ibuprofen. synthetic yield. Because the acid chloride group in 2-chloropropionyl chloride can be hydrolyzed, the results obtained by direct detection are unstable, and the acid chloride group has very strong oxidative and corrosive properties, which is easy to cause damage to the testing instrument. Patent CN1090...

Claims

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Application Information

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Patent Type & Authority Patents(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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