Method for detecting concentration of active components in Grignard reagent solution

A technology of Grignard reagent and active ingredient, which is applied in the field of detection of active ingredient concentration in Grignard reagent solution, can solve the problem that the concentration of active ingredient is not easy to be accurately detected, and can solve the problem that the concentration of active substance cannot be effectively detected, improve the promotion potential and Application prospect, effect of wide range of substrates

Inactive Publication Date: 2019-01-04
河北百灵威超精细材料有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of detection method of active ingredient concentration in the Grignard reagent solution, which can solve the technical problem that the active ingredient concentration in the Grignard reagent solution is not easy to detect accurately

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  • Method for detecting concentration of active components in Grignard reagent solution

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example 1

[0040] Example 1 The detection method of the concentration of active ingredients in THF solution of ethylmagnesium bromide

[0041] Using iodine as an initiator, bromoethane (218g, 2mol) in tetrahydrofuran (500mL) was added dropwise to tetrahydrofuran (500mL) containing magnesium chips (57.6g, 2.4mol), and the reaction prepared tetrahydrofuran of ethylmagnesium bromide solution. Among them, the concentration of active ingredients in the product is roughly estimated to be below 2.0 mol / liter.

[0042] Step 1, prepare benzaldehyde standard solution, dissolve the benzaldehyde purified by distillation in dry THF, and obtain the concentration of benzaldehyde THF solution as 1.0 mol / liter;

[0043] Step 2, under a nitrogen atmosphere, measure 10 mL of the above-mentioned 1 mol / L benzaldehyde tetrahydrofuran solution, add dropwise 4 mL of the prepared ethylmagnesium bromide tetrahydrofuran solution; after reacting for 6 hours, add 10 mL of water as a quenching agent, to obtain reac...

example 2

[0050] The detection method of the active ingredient concentration of the ether solution of example 2 phenylmagnesium iodide

[0051] The ether solution (700mL) of iodobenzene (204g, 1mol) was added dropwise to ether (300mL) containing magnesium chips (28.8g, 1.2mol) to prepare the ether solution of phenylmagnesium iodide. The concentration of active ingredients in the product is roughly estimated to be below 1 mole / liter.

[0052] Step 1, preparing 4-methoxybenzaldehyde standard solution, dissolving the purified 4-methoxybenzaldehyde in distilled ether in dry ether to obtain a concentration of 4-methoxybenzaldehyde solution of 1.0 mol / liter;

[0053] Step 2, measure the ether solution of the above-mentioned 1 mol / liter 4-methoxybenzaldehyde of 10mL, dropwise add the ether solution of phenylmagnesium iodide prepared by 8mL therein; after reacting for 6 hours, add 10mL of methanol as a quenching Killing agent, obtain reaction solution 1;

[0054] Step 3, measure 10 mL of the ...

example 3

[0060] Example 3 Detection method of active ingredient concentration in tetrahydrofuran solution of ethynylmagnesium bromide

[0061] Add acetylene gas to the newly prepared 0.6M butylmagnesium bromide tetrahydrofuran solution to prepare a tetrahydrofuran solution of ethynylmagnesium bromide. The concentration of active ingredients in the product is roughly estimated to be below 0.6 mol / liter.

[0062] Step 1, preparation of benzaldehyde standard solution, the benzaldehyde purified by distillation is dissolved in dry tetrahydrofuran to obtain a concentration of benzaldehyde solution of 1.0 mol / liter;

[0063] Step 2, under a nitrogen atmosphere, measure 10 mL of the above-mentioned 1 mol / L benzaldehyde tetrahydrofuran solution, add dropwise 8 mL of the prepared ethynylmagnesium bromide tetrahydrofuran solution; after reacting for 6 hours, add 10 mL of water as a quenching agent, to obtain reaction solution 1;

[0064] Step 3, under a nitrogen atmosphere, measure 10 mL of the...

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Abstract

The invention discloses a method for detecting the concentration of active components in a Grignard reagent solution. The method comprises the steps that 1, a standard aldehydes solution is prepared;2, a standard aldehydes solution is measured, the solution, in a first solvent, of a Grignard reagent is dropwise added into the standard aldehydes solution for a reaction for n hours, and then a quenching agent is added to obtain a first reaction solution; 3, a standard aldehydes solution is measured, the first solvent is dropwise added into the standard aldehydes solution, after n hours, a quenching agent is added to obtain a second reaction solution; 4, the first reaction solution and the second reaction solution which are equal in volume are selected and subjected to chromatographic detection under same detection conditions respectively, wherein the peak areas corresponding to aldehydes materials in the first reaction solution and aldehydes materials in the second reaction solution respectively are denoted as S1 and S2 respectively; 5, according to a computational formula, the concentration M of the active components in the solution, in the first solvent, of the Grignard reagent isobtained, wherein the computational formula is an equation, namely M=(1-S1 / S2)*X1*V1 / V2 mol / L. By means of the method, the technical problem can be solved that the concentration of the active components in the Grignard reagent solution is difficult to accurately detect.

Description

technical field [0001] The invention relates to a method for detecting the concentration of active components in a Grignard reagent solution. Background technique [0002] Grignard reagents, also known as organomagnesium compounds, refer to the general term for substances in which carbon elements in organic groups (such as alkyl groups and aromatic groups) are directly combined with magnesium atoms. These compounds usually have high reactivity and are widely used in Organic chemistry, polymer chemistry, material chemistry, life science and other fields. Such reagents are often stored in the form of solutions, which are convenient for storage and use. The solvents used are often selected from alkane compounds, ether compounds, and the like. [0003] Grignard reagents are usually strongly alkaline and are prone to quenching reactions with acidic substances, water, and even alcohols. After reacting with water and alcohols, the resulting substance still shows strong alkalinity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 范玉凯刘文彬刘云生
Owner 河北百灵威超精细材料有限公司
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