Synthetic method of important intermediate of hexythiazox
A synthesis method and intermediate technology are applied in the field of preparation of important intermediates of pesticide technical materials, which can solve the problems of high price and low yield of raw and auxiliary materials, and achieve the effects of low cost, high yield and high content.
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Embodiment 1
[0029] 1) Put 91.0g of 98.9% lactic acid into the reaction kettle, without stirring at this time, first raise the temperature to 53-55°C, after the lactic acid melts, stir slowly, add 150.0g of thionyl chloride dropwise, and finish the reaction After 2-3 hours, excess thionyl chloride was removed to obtain intermediate I;
[0030] 2) Put 113.0g of chlorobenzene, 150.0g of anhydrous aluminum trichloride and 300.0g of dichloromethane into the reaction kettle, cool down to 10-30°C, drop all the intermediates I prepared above and react for 5-8h, Add 200 g of ice water to quench the reaction, separate the phases, and evaporate dichloromethane to dryness to obtain intermediate II;
[0031] 3) Put intermediate II, 55g of ammonium chloride, 3g of catalyst and 250g of dimethyl sulfoxide into the pressurized reactor, raise the temperature to 110-150°C, keep it warm for 5-8h, and cool down to 10- Evaporate dimethyl sulfoxide to dryness at 30°C to obtain the crude product of 2-amino-1-(p...
Embodiment 2
[0034] 1) Put 91.00g of 98.9% lactic acid into the reaction kettle, do not stir at this time, first raise the temperature to 53-55°C, after the lactic acid melts, stir slowly, add 142.80g of thionyl chloride dropwise, and finish the reaction 2 -3 hours, remove excess thionyl chloride to obtain intermediate I;
[0035] 2) Put 112.50g of chlorobenzene, 146.85g of anhydrous aluminum trichloride and 225.00g of dichloromethane into the reaction kettle, cool down to 10-30°C, drop all the intermediates I prepared above and react for 5-8h, Add 168.75 g of ice water to quench the reaction, separate the phases, and evaporate dichloromethane to dryness to obtain intermediate II;
[0036] 3) Put intermediate II, 53.50g of ammonium chloride, 0.92g of catalyst and 239.85g of dimethyl sulfoxide into the pressurized reactor, raise the temperature to 110-150°C, keep it warm for 5-8h, and cool down after passing the central control To 10-30°C, evaporate dimethyl sulfoxide to dryness to obtain ...
Embodiment 3
[0039] 1) Put 91.00g of 98.9% lactic acid into the reaction kettle, without stirring for now, first raise the temperature to 53-55°C, after the lactic acid melts, stir slowly, add 178.50g of thionyl chloride dropwise, and finish the reaction 2 -3 hours, remove excess thionyl chloride to obtain intermediate I;
[0040] 2) Put 123.75g of chlorobenzene, 160.20g of anhydrous aluminum trichloride and 495.00g of dichloromethane into the reaction kettle, cool down to 10-30°C, drop all the intermediates I prepared above and react for 5-8h, Add 371.25 g of ice water to quench the reaction, separate the phases, evaporate dichloromethane to dryness, and obtain intermediate II;
[0041] 3) Put intermediate II, 58.85g of ammonium chloride, 9.23g of catalyst and 479.70g of dimethyl sulfoxide into the pressurized reactor, raise the temperature to 110-150°C, keep it warm for 5-8h, and cool down after passing the central control To 10-30°C, evaporate dimethyl sulfoxide to dryness to obtain th...
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