Methylation synthesis method based on pyraclostrobin intermediate
A technology for pyraclostrobin and intermediates, which is applied in the field of organic compound synthesis, can solve the problems of unsuitability for large-scale industrialization, great harm to the human body and the environment, and high cost, so as to reduce production costs and reduce environmental pressure. , the effect of reducing environmental pressure
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Embodiment 1
[0048]This embodiment relates to pyraclostrobin intermediate The methylation synthesis method performed.
[0049] The process steps are as follows:
[0050] 1) Add the pyraclostrobin intermediate, phase transfer catalyst, solvent, and alkali solution into the autoclave, and replace the gas in the autoclave with methylene chloride gas.
[0051] The phase transfer catalyst is tetrabutylammonium chloride.
[0052] The solvent is selected from a water-insoluble organic solvent, such as a mixture of dichloroethane selected from halogenated alkanes, chlorobenzene selected from aromatic hydrocarbons, and methyl tert-butyl ether selected from ethers.
[0053] The alkaline solution is 20% sodium hydroxide aqueous solution.
[0054] Control the mass ratio of pyraclostrobin intermediate to the selected phase transfer catalyst and solvent at 1:0.01:20; control the equivalent ratio with alkali and methylene chloride gas at 1:2:1.
[0055] 2) The temperature is controlled at 10°C, and ...
Embodiment 2
[0058] This embodiment relates to pyraclostrobin intermediate The methylation synthesis method performed.
[0059] The process steps are as follows:
[0060] 1) Add the pyraclostrobin intermediate, phase transfer catalyst, solvent, and alkali solution into the autoclave, and replace the gas in the autoclave with methylene chloride gas.
[0061] The phase transfer catalyst is selected from benzyltriethylammonium bromide and PEG800.
[0062] The solvent is an organic solvent miscible with water, such as methanol, ethanol, etc. selected from esters.
[0063] The alkaline solution is an aqueous solution composed of lithium hydroxide, lithium carbonate and sodium hydroxide with a concentration of 5%.
[0064] Control the mass ratio of pyraclostrobin intermediate to the selected phase transfer catalyst and solvent at 1:0.2:1; control the equivalent ratio with alkali and methylene chloride gas at 1:3:5.
[0065] 2) The temperature is controlled at 95°C, and the pressure of the m...
Embodiment 3
[0068] This embodiment relates to pyraclostrobin intermediate The methylation synthesis method performed.
[0069] The process steps are as follows:
[0070] 1) Add the pyraclostrobin intermediate, phase transfer catalyst, solvent, and alkali solution into the autoclave, and replace the gas in the autoclave with methylene chloride gas.
[0071] The phase transfer catalyst is selected from benzyl triethyl ammonium chloride.
[0072] The solvent is selected from water-insoluble organic solvents, such as chlorobenzene or dichlorobenzene selected from (halogenated) aromatic hydrocarbons.
[0073] The alkaline solution is 40% sodium hydroxide aqueous solution.
[0074] The mass ratio of the pyraclostrobin intermediate to the phase transfer catalyst and solvent selected above is controlled at 1:0.02:5; the equivalent ratio to the alkali and methylene chloride gas is controlled at 1:1.4:2.
[0075] 2) The temperature is controlled at 80°C, and the pressure of the monochlorometha...
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