A kind of preparation method of fenfentrazone intermediate
A technology of fenfentrazone and its intermediates, which is applied in the field of preparation of 2,3-dimethyl-4-methylsulfonylbromobenzene, an intermediate of fenfentrazone, can solve improper operation of peracetic acid and explosion accidents and other issues, to achieve the effect of improved reaction safety, less environmental pollution, and mild reaction conditions
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Embodiment 1
[0037] Dissolve 51.0g (0.333mol) of 2,3-dimethylanisole in 150g of 1,2-dichloroethane, add 67.4g (0.399mol) of hydrobromic acid aqueous solution with a concentration of 48% by mass, Then add 0.5g (0.00375mol) aluminum trichloride and 1g (0.003mol) sodium tungstate, start stirring, and start to drop 97.0g (0.999mol) of hydrogen peroxide with a mass percentage concentration of 35% at 20-30°C, about The dropwise addition was completed in 1 hour, and the mixture was heated to 50° C. for 3 hours, and a large amount of solid was precipitated. Suction filtration under reduced pressure, rinse the filter cake with an appropriate amount of 1,2-dichloroethane, and dry to obtain 70.2 g of 2,3-dimethyl-4-methylsulfonylbromobenzene, with a GC purity of 98.1% and a yield of 78.6 %.
Embodiment 2
[0039] Dissolve 51.0g (0.333mol) of 2,3-dimethylanisole in 200g of methanol, add 67.4g (0.399mol) of hydrobromic acid aqueous solution with a mass percent concentration of 48%, and then add 0.5g (0.00375 mol) aluminum trichloride and 1g (0.003mol) sodium tungstate, start stirring, start dropwise adding 97.0g (0.999mol) of hydrogen peroxide with a mass percentage concentration of 35% at 20-30°C, and drop it in about 1 hour. After the addition, it was heated to 50° C. for 3 hours, and a large amount of solid was precipitated. After suction filtration under reduced pressure, the filter cake was rinsed with an appropriate amount of methanol and dried to obtain 70.5 g of 2,3-dimethyl-4-methylsulfonylbromobenzene, with a GC purity of 98.5% and a yield of 79.3%.
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