Synthesis process of primisulfuron-methy and other fluoric hebicide
A technology for fluoxulfuron-methyl and herbicides is applied in the field of synthesizing fluorine-containing herbicides, which can solve the problems of low yield and ozone layer destruction in the synthesis method, and achieve the effects of improving the yield and protecting the atmospheric environment.
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[0012] Embodiment: For the key intermediate 2-amino of synthetic flurimsulfuron methyl, the reaction of 4,6 bis (difluoromethoxy) pyrimidines:
[0013] The specific operation is as follows, 1.27g (0.01mol) of 2-amino, 4,6-dihydroxypyrimidine, 0.007mol of Cu + catalyst while adding 30ml of CH 3 CN was used as a solvent, put it into the reflux tube and a thermometer, filled with nitrogen gas protection, added dropwise 4.5g (0.025mol) fluorosulfone difluoroacetic acid, raised the temperature to 50°C, and reacted for 3 hours. After the reaction was completed, filter, and evaporate the filtrate to its solvent. After cooling, a solid was precipitated, and the resulting solid was washed with 5% NaOH solution to obtain a crude product, which was separated by column chromatography (developing solvent: V (petroleum ether): V (ethyl acetate) = 5: 1) to obtain a white needle. 0.4 g of solid crystals, yield 18%. The obtained crystals were examined: m.p, 68~69°C; H-NMR, δ: (CDCl 3 / TMS...
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