Preparation method of picoxystrobin

[0053] Add 160g sodium hydroxide aqueous solution (10%w / w), 36.7g 2-chloro-6-trifluoromethylpyridine (content 99%) in 500mL stainless steel autoclave, close still cover, oil bath is heated up to 150 ℃, The pressure of the kettle is 0.4MPa, after stirring and reacting for 5 hours, remove the heat source, take a sample, and control in the high performance liquid chromatography (condition: Agilent ZORBAX Eclipse XDB-C18, 4.6*250*5μm; mobile phase: methanol: 0.1% phosphoric acid = 55:45 (V:V); flow rate: 1.0mL / min; wavelength: 254nm), the central control spectrum is as follows figure 1 shown. After the reaction was complete, the pressure relief valve was opened, the reaction solution was cooled to 5° C., filtered and drained, the wet weight of the filter cake was 37.3 g, and the content was 92.7% by the external standard method (using 2-hydroxyl-6-trifluoromethylpyridine Sodium salt), the separation yield is 93.4%.

[0054] Add 37.3g of 2-hydroxyl-6-trifluoromethylpyridine sodi

[0057] Add 40g aqueous sodium hydroxide solution (20% w / w), 33.7g 2-fluoro-6-trifluoromethylpyridine (content 98%), and 1.5g tetrabutylammonium bromide into a 250mL stainless steel autoclave. Close the lid of the kettle, raise the temperature of the oil bath to 160°C, and the pressure of the kettle to 1.2MPa. After stirring and reacting for 10 hours, remove the heat source, take a sample, and control in the high performance liquid chromatography (condition: Agilent ZORBAX Eclipse XDB-C18, 4.6*250*5μm; flow Phase: methanol: 0.1% phosphoric acid = 55:45 (V:V); flow rate: 1.0 mL / min; wavelength: 254 nm). After the reaction was complete, the pressure relief valve was opened, the reaction solution was cooled to 10°C, filtered and drained, the wet weight of the filter cake was 44.6g, and the content was 79.4% detected by the external standard method (with 2-hydroxyl-6-trifluoromethylpyridinium sodium Salt meter), the separation yield is 94.9%.

[0058] Add 44.6g of 2-hydroxyl-6-tr

[0060] In 250mL stainless steel autoclave, add 60g sodium hydroxide aqueous solution (40%w / w), 36.7g 2-chloro-6-trifluoromethylpyridine (content 99%), close still lid, oil bath is heated up to 140 ℃, The pressure of the kettle is 0.35MPa, after stirring and reacting for 3 hours, remove the heat source, take a sample, and control in the high performance liquid chromatography (condition: Agilent ZORBAX Eclipse XDB-C18, 4.6*250*5μm; mobile phase: methanol: 0.1% phosphoric acid = 55:45 (V:V); flow rate: 1.0 mL / min; wavelength: 254 nm). After the reaction is complete, open the pressure relief valve, cool the reaction solution to 10°C, filter and drain, the wet weight of the filter cake is 38.1g, and the content is 92.8% by the external standard method (with 2-hydroxyl-6-trifluoromethylpyridinium sodium Salt meter), the separation yield is 95.6%.

[0061] In a 500mL three-necked flask, add 38.1g of the wet product of 2-hydroxy-6-trifluoromethylpyridine sodium salt obtained in the