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Preparation method of impurities in metalaxyl-M

A technology for refining mefenaxyl and impurities, applied in the field of pesticide analysis, can solve problems such as less research, and achieve the effect of simple operation, strong versatility, and economical feasibility

Active Publication Date: 2019-03-12
HANGZHOU POOKE TESTING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

FAO also stipulates the limit of 4-methoxy-5-methyl-5H-1,2-oxazolidine 2,2-dioxide, a related impurity of metalaxyl, which has been tested by high performance liquid chromatography and Qualitative and quantitative research on the original drug of mefenaxyl by liquid chromatography-mass spectrometry, but there are few studies on this related impurity, especially in the synthesis or preparation process

Method used

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  • Preparation method of impurities in metalaxyl-M
  • Preparation method of impurities in metalaxyl-M
  • Preparation method of impurities in metalaxyl-M

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the preparation of impurity

[0026] S1: Weigh 100g of metalaxyl, and use liquid chromatography to measure the normalized content of related impurities to be 0.12%. The collected eluate is chromatographed on a 100-200 mesh silica gel Thin-layer chromatography has been used for detection. The developer is a mixed solvent of petroleum ether and ethyl acetate with a volume ratio of 20:1. The main component of metalaxyl is R f The value is located at 0.3-0.5. When the first section of eluent is used for elution, the eluent before the main component of metalaxyl is not detected is collected as the first section of eluent. When the thin layer chromatography starts After the main component of Nafaxyl was detected, the second stage of eluent was used for elution, and the eluate obtained from the time when the main component of Nafaxyl began to flow out to when the main component of Nafaxyl could not be detected was collected as the second eluent. The second secti...

Embodiment 2

[0030] Example 2: Verification of structure

[0031] The impurity product that makes in embodiment 1 is carried out nuclear magnetic field and mass spectrometry analysis, and its spectrogram is as Figure 1-3 shown.

[0032] Proton NMR spectroscopy (BRUKER AV-400 nuclear magnetic resonance instrument, CDCl 3 )

[0033] 1 H-NMR: δppm 5.80 (CHCH 3 , d, J=0.8Hz s, 1H), 5.12-5.07(C=CH, m, 1H), 3.86(OCH 3 ,s,3H),1.58(CHCH 3 , d, J=6.8Hz, 3H).

[0034] Carbon NMR spectroscopy (BRUKER AV-400 nuclear magnetic resonance instrument, CDCl 3 )

[0035] 13 C-NMR: δppm 168.76, 93.93, 78.65, 59.86, 18.44.

[0036] Mass spectrometry (Waters ZQ2000, solvent methanol, ESI (+) 70V)

[0037] [M+H] obtained from mass spectrum ESI(+) results + The m / z value of is 164.9.

[0038] from 1 From the H-NMR data, it can be seen that the molecule contains 1 -CH-CH 3 , 1 C=CH, 1 -O-CH 3 ,from 13 C-NMR data can infer that the molecule contains 5 different types of carbon atoms, and then comb...

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Abstract

The invention provides a preparation method of impurities in metalaxyl-M, and belongs to the technical field of pesticide analysis. According to the preparation method, the impurities in metalaxyl-M original medicine are enriched through means of silica gel column chromatography and decompression concentration, and then the metalaxyl-M impurities, namely 4-methoxy-5-methyl-5H-1, 2-oxazolidine 2, 2-dioxide, are separated and purified through preparative liquid chromatography. The purity of the 4-methoxy-5-methyl-5H-1, 2-oxazolidine 2, 2-dioxide impurities in a product prepared by the inventionis high and reaches 98.24%, the preparation method can be used for qualitative and quantitative analysis of the impurities in the metalaxyl-M, the important effect on quality control over the metalaxyl-M is achieved, and the preparation method is economical, feasible, easy to operate and high in universality.

Description

technical field [0001] The invention belongs to the technical field of pesticide analysis, and in particular relates to a method for preparing impurities in mefenaxyl. Background technique [0002] Metalaxyl is an amide fungicide developed by Syngenta, also known as high-efficiency metalaxyl, which has preventive and therapeutic effects. It is effective against vegetables, fruit trees, and tobacco caused by downy mildew, phytophthora, and pythium. , cotton and other crop diseases have a good control effect. The substance has a fast degradation rate in soil, a long duration of action, less spraying times, is safe for users, and has good compatibility with the environment. In pesticide export registration and international trade, governments of various countries are very concerned about the types and concentrations of related impurities in pesticide raw materials and preparations, and related impurities are mandatory inspection items, such as 4-methoxy-5-methyl-5H-1, 2-Oxazo...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 徐锦忠王剑田婷刘朝
Owner HANGZHOU POOKE TESTING TECH CO LTD