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A high-efficiency cyhalothrin and cyclochlorofluoroester technology is applied in the field of pesticides, and can solve the problems of long synthesis process route, high industrialization cost, hindering product development, etc., and achieves reduction of industrialization cost, improvement of reaction efficiency, and improvement of process technology. Effect
Inactive Publication Date: 2009-05-20
JIANGSU HUANGMA AGROCHEM
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The product is prepared through processes such as addition, cyclization, elimination of hydrolysis, separation, acyl chloride, esterification, and epimerization. The synthesis process route is long, and the reaction efficiency in the esterification reaction is low, and the industrialization cost Relatively high, which hinders the development of the product
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Embodiment 1
[0014] A kind of efficient cyhalothrin its production technology is
[0015] 1), layering---reaction raw materials are methyl peritinate and trichlorotrifluoroethane;
[0016] 2), cyclization --- the reaction raw materials are tert-butanol, chlorofluoroester and sodium tert-butoxide, and the reaction is precipitated and distilled to obtain chlorofluoroester;
[0017] 3), eliminate hydrolysis --- the reaction raw material is potassium hydroxide and the chlorofluoroester obtained by the cyclization reaction of the above step 3), and the reaction is prepared by precipitation, hydrolysis, separation, and filtration to obtain 2-cis-chlorofluorochroic acid ;
[0018] 4), acid chlorination---reaction raw materials are thionyl chloride, toluene and step 3) eliminating the 2-cis-chlorofluorochrysanthemum acid obtained by the hydrolysis reaction, and obtaining chlorofluorochrysanthemum acid chloride through precipitation and distillation;
[0019] 5), esterification --- the reaction r...
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Abstract
The invention relates to an efficient cyhalothrin and a manufacturing technology thereof, the manufacturing technology is as follows: (1) layer addition-reaction materials are 3, 3-dimethyl-4-pentenoic acid methyl ester and trichlorotrifluoroethane; (2) cyclization- reaction materials are tertiary butyl alcohol, Bifenthrin and sodium tert-butoxide; (3) elimination of hydrolysis-reaction materials are potassium hydroxide and cyclic Bifenthrin, and by exsolution, hydrolysis, separation and filtration 2-cis-3-(2-chloro-3, 3, 3-trifluro-1-propenyl)-2, 2-dimethyl cyclopropane carboxylic acid can be prepared; (4) chloroformylation-reaction materials are thionyl chloride, methylbenzene and 2-cis-3-(2-chloro-3, 3, 3-trifluro-1-propenyl)-2, 2-dimethyl cyclopropane carboxylic acid, and by exsolution and distillation, 3-(2-chloro-3, 3, 3-trifluoro-1-propenyl)-2, 2-dimethylcyclopropane carbonyl chloride is obtained; (5) esterification- reaction materials are phenylate aldehyde, sodium cyanide, PTC and 3-(2-chloro-3, 3, 3-trifluoro-1-propenyl)-2, 2-dimethylcyclopropane carbonyl chloride, by water rinse, exsolution and distillation, the cyhalothrin is prepared; and (7) epimerization-inoculating crystal is added for carrying out an epimerization reaction, and after the reaction, an end product-the efficient cyhalothrin is obtained by filtration and drying. As the invention adopts the technical proposal, the efficient cyhalothrin prepared by the invention greatly shortens the technological route and obviously improves the reaction efficiency through the improvement of technical skills, thereby reducing the cost of industrialization.
Description
technical field [0001] The invention relates to a pesticide, especially a kind of efficient cyhalothrin. Background technique [0002] Lambda-cyhalothrin is a patented product first successfully developed by the British ICI company in 1982 (the current patent protection period has expired). The product is prepared through processes such as addition, cyclization, elimination of hydrolysis, separation, acyl chloride, esterification, and epimerization. The synthesis process route is long, and the reaction efficiency in the esterification reaction is low, and the industrialization cost Relatively high, hindering the development of this product. Contents of the invention [0003] In view of the above-mentioned shortcomings, the present invention provides a kind of efficient cyhalothrin, through the improvement of the process technology, the process route is shortened, and at the same time, a new catalyst is used in the esterification reaction to improve the reaction efficiency...
Claims
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