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Synthesis method for stable isotope labeled leucomalachite green

A leuco-malachite green and stable isotope technology, which is used in the preparation of imino compounds, the preparation of amino compounds from amines, organic chemistry, etc. Malachite green and leuco-malachite green, the method is cumbersome and other problems, to achieve good economy and use value, stable atomic utilization, simple method and process.

Inactive Publication Date: 2012-11-28
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance liquid chromatography has high sensitivity, but this method is cumbersome, and the total amount of malachite green is measured, and malachite green and leuco malachite green cannot be quantitatively determined separately, so this method is rarely used.
Thin-layer chromatography is simple and quick to operate, but it cannot detect malachite green and leuco malachite green at the same time
Spectrophotometry has high detection limits, but low sensitivity and poor accuracy of detection

Method used

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  • Synthesis method for stable isotope labeled leucomalachite green
  • Synthesis method for stable isotope labeled leucomalachite green
  • Synthesis method for stable isotope labeled leucomalachite green

Examples

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Embodiment 1

[0029] an isotope 13 The synthetic method of C mark leuco malachite green, this method specifically comprises the following steps:

[0030] the isotope 13 C-labeled N,N-dimethylaniline- 13 C 2 Mix it with benzaldehyde at a molar ratio of 2:1, and with urea at a molar ratio of 2:1, then place it in acetic acid, control the reaction temperature at 90°C, and stir for 6 hours to obtain 13 C-marked leuco malachite green is the product with a chemical purity of 99.1% and an isotopic abundance of 99.2% atom.

[0031] owned 13 The leuco malachite green marked by C can be further oxidized to obtain malachite green, which will 13 C-marked leuco malachite green is placed in a mixed solution of acetic acid and acetic anhydride, and then FeCl is added 3 , FeCl 3 and 13 The weight ratio of C-labeled leuco malachite green is 0.04:1, under the nitrogen and oxygen atmosphere, the reaction temperature is controlled at 70°C, and the reaction is stirred for 8h to obtain 13 C-labeled mala...

Embodiment 2

[0033] an isotope 13 The synthetic method of C mark leuco malachite green, this method specifically comprises the following steps:

[0034] the isotope 13 C-labeled N,N-dimethylaniline- 13 C 2 It is mixed with paraformaldehyde in a molar ratio of 3:1, and benzaldehyde in a molar ratio of 3:1, and then placed in an acetonitrile solution. The reaction temperature is controlled at 120°C, and the reaction is stirred for 4 hours to obtain 13 C-marked leuco malachite green is the product with a chemical purity of 99.0% and an isotopic abundance of 99.3% atom.

[0035] owned 13 The leuco malachite green marked by C can be further oxidized to obtain malachite green, which will 13 C-labeled leuco malachite green is placed in acetone solution, then CuCl is added, CuCl and 13 The weight ratio of C-marked leuco malachite green is 0.1:1, under nitrogen and oxygen atmosphere, the reaction temperature is controlled at 50°C, and the reaction is stirred for 6h to obtain 13 C-labeled mal...

Embodiment 3

[0037] an isotope 15 The synthetic method of N mark leuco malachite green, this method specifically comprises the following steps:

[0038] the isotope 15 N-labeled N,N-dimethylaniline- 15 The molar ratio of N to benzaldehyde is 3:1, mixed with paraformaldehyde at a molar ratio of 4:1, then placed in acetic anhydride, the reaction temperature is controlled at 160°C, and the reaction is stirred for 4 hours to obtain 15 N-labeled leuco malachite green is the product with a chemical purity of 99.5% and an isotopic abundance of 99.2% atom.

[0039] owned 15 N-labeled leuco malachite green can also be further oxidized to obtain malachite green, which will 15 N-labeled leuco malachite green was placed in acetic acid solution, then CuCl was added, CuCl and 15 The weight ratio of N-labeled leuco malachite green is 0.06:1, under the nitrogen and oxygen atmosphere, the reaction temperature is controlled at 90°C, and the reaction is stirred for 6h to obtain 15 N-labeled malachite gre...

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Abstract

The invention relates to a synthesis method for stable isotope labeled leucomalachite green. The stable isotope labeled leucomalachite green is obtained by reacting stable isotope labeled N, N-dimethylaniline with benzaldehyde. Compared with the prior art, after the stable isotope labeled leucomalachite green prepared by the method and malachite green are separated and purified, the chemical purity reaches over 99 percent and the isotope abundance is over 98 percent atom.

Description

technical field [0001] The invention relates to the field of isotope labeling, in particular to a synthesis method for isotope internal standard detection reagent stable isotope labeling leuco malachite green and malachite green. Background technique [0002] Leuco malachite green, malachite green and other triphenylmethane compounds have been widely used in fish farming as fungicides. Leuco malachite green and triphenylmethane, a chemical functional group in malachite green, can cause cancer. Many countries have banned them, but fishermen still use them to prevent fungal infections in fish, and some transporters use them as disinfectants to prolong fish life. Survival time in long-distance trafficking. In order to prevent leuco malachite green, malachite green and other triphenylmethane residues from entering the food chain, farmers and government monitoring departments need a fast, accurate and sensitive technology to detect it. [0003] The main detection techniques use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/50C07C209/68C07C251/30C07C249/02
Inventor 杨超杨维成罗勇李美华
Owner SHANGHAI RES INST OF CHEM IND
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