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High performance liquid chromatography detection method of 3,4,5-trifluorophenylboronic acid

A technology of high performance liquid chromatography and trifluorobenzene boric acid, applied in the field of chemical analysis, can solve the problems of lack of analysis standards, hindering product promotion and application, etc.

Inactive Publication Date: 2015-12-23
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This makes the product without a unified analysis standard, which hinders the promotion and application of the product

Method used

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  • High performance liquid chromatography detection method of 3,4,5-trifluorophenylboronic acid
  • High performance liquid chromatography detection method of 3,4,5-trifluorophenylboronic acid
  • High performance liquid chromatography detection method of 3,4,5-trifluorophenylboronic acid

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Experimental program
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Effect test

Embodiment 1

[0014] 1. Instrument: Agilent 1260A--high performance liquid chromatography, electronic balance

[0015] 2. Determination method:

[0016] Accurately weigh 50 mg of the sample, place it in a 2ml sample bottle, add mobile phase, ultrasonically dissolve and dilute to the mark, shake well, and use it as the test solution; use octadecyl bonded silica gel as the packed column, and the mobile phase is composed of 5 mmol phosphoric acid The solution and acetonitrile were prepared at a volume ratio of 60:40; the 5mmol phosphoric acid solution was prepared by adding 0.576g of phosphoric acid (reagent), adding 1000ml of water and shaking well. The detection wavelength is 254nm, and the flow rate is 1.0ml / min. Get need testing solution 8ul and inject in the liquid chromatograph, record chromatogram to main peak retention time 6 times.

Embodiment 2

[0018] 1. Instrument: Agilent 1260A--high performance liquid chromatography, electronic balance

[0019] 2. Determination method:

[0020] Preparation of standard solution: Accurately weigh 50 mg, 100 mg, and 150 mg of 3,4,5-trifluorophenylboronic acid standard into 25 ml volumetric flasks, dissolve and dilute to the mark with mobile phase, shake well, and use as standard solution for later use.

[0021] Standard curve: Take the above-mentioned 3 concentrations of standard solution for one injection, inject 2 injections of each standard solution, record the spectrum, and make a weight / peak area logarithmic curve. Correlation coefficient ≥ 0.999.

[0022] Preparation of sample solution: Accurately weigh 100 mg of sample, put it in a 25ml measuring bottle, add mobile phase to ultrasonically dissolve and dilute to the mark, shake well, and use it as the test solution; use octadecyl bonded silica gel as the filling column, and the mobile phase is composed of 5mmol phosphoric aci...

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Abstract

The invention discloses a high performance liquid chromatography detection method of 3,4,5-trifluorophenylboronic acid, and belongs to the technical field of chemical analysis. According to the high performance liquid chromatography detection method, octadecyl silane is taken as a packed column, distilled water-acetonitrile is taken as a mobile phase, and phosphoric acid is added into the mobile phase. The high performance liquid chromatography detection method can be used for accurate analysis and determination of the content of 3,4,5-trifluorophenylboronic acid and related substances, effective control of the quality of 3,4,5-trifluorophenylboronic acid in practical production processes, and providing construction of universal standards of the product with foundation.

Description

Technical field: [0001] The invention relates to the technical field of chemical analysis, in particular to a high performance liquid chromatography detection method for 3,4,5-trifluorophenylboronic acid. Background technique: [0002] Fluorine-containing phenylboronic acid is a kind of organic synthesis, pharmaceutical and chemical intermediates that are relatively stable in the air, insensitive to moisture, can be stored for a long time and have high reactivity. The Suzuki coupling reaction of fluorine-containing phenylboronic acid and halogenated aromatic hydrocarbons has good position selectivity and stereoselectivity, various chemical functional groups do not change during the reaction, the reaction conditions are mild, and the yield is high. important way. Fluorine-containing phenylboronic acid has a very important application in organic synthesis reactions such as the formation of C—O bonds, C—N bonds, and C—S bonds. Fluorine-containing phenylboronic acid is a fluor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杨青赵士民汪洪湖陈毛毛
Owner BENGBU CHINA SYNCHEM TECH CO LTD
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