Purifying method of propoxur
A purification method, propoxur technology, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve problems such as difficult to achieve purification effect, unpleasant special smell, etc., achieve white color, avoid decomposition, and simple operation Effect
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[0027] Example 1:
[0028] A 500mL three-necked flask with cooling tube, thermometer, and stirring was added 214.4g of propoxur (97.5%) and 8.5g of petroleum ether, stirred and heated to 95℃ to completely melted, and controlled the temperature of the system to slowly drop to 85℃ (cooling rate 0.1℃ / min) and maintain for 1h, stand still to crystallize. A small amount of yellow liquid appeared in the kettle floating above the white solid, which was removed from the system. The white solid is heated and melted and sliced to obtain 205.2g of white, odorless Proxacarb (liquid chromatography, external standard) with a content of 99.3%. The yield is 97.5%. The mass of the yellow liquid removed from the system was 15.8 g, which was analyzed to be a 32.5% petroleum ether solution of propoxur, and 1,2-diisopropoxybenzene and 1-isopropoxy-2-methoxybenzene were also dissolved. Simple distillation can recover 6g of petroleum ether, and the remaining oily paste residue after distillation c...
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[0029] Example 2
[0030] Add 214.4g of procarb (97.5%) and 6g of petroleum ether to a 500mL three-necked flask with cooling tube, thermometer and stirring, stir and heat to 100℃ to completely melt, control the temperature of the system to slowly drop to 90℃ (cooling rate 0.1℃ / min ) And maintain for 1h, stand still to crystallize. A small amount of yellow liquid appeared in the kettle floating above the white solid, which was removed from the system. The white solid was heated and melted and then sliced to obtain 206.5g of white, odorless Proxacarb (liquid chromatography, external standard) with a content of 99.1%. The yield was 97.9%. The mass of the yellow liquid removed from the system was 12.0 g, which was analyzed to be a petroleum ether solution of 36.2% propoxur, and 1,2-diisopropoxybenzene and 1-isopropoxy-2-methoxybenzene were also dissolved. 3g of petroleum ether can be recovered by simple distillation, and the remaining oily paste residue after distillation can be ...
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[0031] Example 3
[0032] A 500mL three-necked flask with cooling tube, thermometer, and stirring was added 214.4g of propoxur (97.5%) and 4.2g of petroleum ether, stirred and heated to 100℃ to completely melted, and controlled the temperature of the system to slowly drop to 85℃ (cooling rate 0.1℃ / min) and maintain for 2h, stand still to crystallize. A small amount of yellow liquid appeared in the kettle floating above the white solid, which was removed from the system. The white solid was heated and melted and sliced to obtain 208.2 g of white, odorless Proxacarb (liquid chromatography, external standard) with a content of 98.8%. The yield was 98.4%. The mass of the yellow liquid removed from the system was 8.4 g, which was analyzed to be a petroleum ether solution of 39.5% propoxur, and 1,2-diisopropoxybenzene and 1-isopropoxy-2-methoxybenzene were also dissolved. 2g of petroleum ether can be recovered by simple distillation, and the remaining oily paste residue after dist...
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