Prepn of etofenprox as pesticide

A technology for etherethrin and insecticide, which is applied in the field of chemical preparation of the pesticide etherethrin, can solve the problems of harsh reaction conditions, high cost of raw materials, and difficulty in industrialization.

Inactive Publication Date: 2004-11-24
SHANGHAI PESTICIDE RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current synthetic method is not very ideal in terms of yield and product content due to harsh reaction conditions.
The high cost of raw materials makes industrialization more difficult, and it is difficult to implement industrialization to achieve large-scale application

Method used

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  • Prepn of etofenprox as pesticide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add (industrial grade) 304 grams (2 mol) of p-tert-butylphenol and 229 grams (2.2 mol) of acid anhydride into a 1000 ml three-necked reaction flask, add 1 mL of inorganic acid, heat and stir, heat up to 130 ° C, react for 8 hours, and reduce The by-product acetic acid and unreacted acetic anhydride were steamed under pressure, the kettle liquid was washed to neutrality, and the layers were separated, and the oil phase was dried to obtain p-tert-butylacetophenone, weighing 384 grams, and the content after analysis was 97%. The rate is 97%.

[0014] Add the prepared p-tert-butylacetophenone (1.94mol) into a 1000ml three-necked reaction flask, add 2g of azobisisobutyronitrile as an initiator, add 450mL of carbon tetrachloride, heat and stir, heat up to 80°C and reflux, Chlorine gas was passed for 3 hours, and the whole reaction was irradiated with a fluorescent lamp. The reaction solution was washed with 600mL of 3% sodium sulfite aqueous solution and separated into layer...

Embodiment 2

[0018] A total of 83.9 grams of unused [4-(2-chloro-1,1-dimethylethyl)phenyl] acetate obtained from the reaction in Example 1 has a content of 98%. A total of 0.364mol of the above-mentioned raw materials, as well as 108 grams (0.9mol) of bromoethane and 82.5 grams of KOH were added to a 500 ml three-necked reaction flask, heated and stirred, and 2.1 grams of benzyltriethylammonium chloride could be dropped in. The reaction temperature was 35 ~45°C, the reaction time is 2 hours, the reaction solution is washed several times with 150mL water and separated, the liquid phase is the product 1-chloro-2-(4-ethoxyphenyl)-2-methylpropane 77.8 grams , crude product content 80.6%, yield 81.3%.

[0019] Add 39.4 grams (0.15mol) of 1-chloro-2-(4-ethoxyphenyl)-2-methylpropane, 33.8 grams (0.16mol) of sodium m-phenoxybenzyloxide into a 250 ml three-necked reaction flask. ), 0.38 grams of tetraethylammonium bromide, 150 milliliters of DMF, heated and stirred, heated up to 120 ° C for 8 hour...

Embodiment 3

[0021] Add 38.4 grams (0.15mol) of the remaining 1-chloro-2-(4-ethoxyphenyl)-2-methylpropane prepared in Example 3 to a 250 ml three-necked reaction flask, 33.8 m-phenoxybenzyl sodium gram (0.16mol), 0.38 gram of tetraethylammonium bromide, 150 milliliters of DMF, heated and stirred, heated up to 140 ℃ and reacted for 16 hours. Purified to obtain 34.1 grams with a content of 82.3%, and a yield of 49.7%.

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Abstract

The present invention belongs to the field of pesticide technology. The preparation of etofenprox as pesticide uses p-tert-butyl phenol as initial material and includes four reaction steps of acetylating, chlorination, oxyethylation, etc. in the presence of catalyst. The present invention has mild reaction condition, low material cost and simple operation and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of pesticides, and in particular relates to a chemical preparation method of the insecticide etofenprox. technical background [0002] Insecticides account for a large proportion of pesticides. In recent years, four highly toxic organophosphorus insecticides, methamidophos, methyl parathion, parathion and monocrotophos, have been widely used in rice, cotton, The pest control of fruit trees and vegetables has reached an annual output of more than 96,500 tons. These highly toxic pesticides have caused human and animal poisoning, environmental pollution, and the negative effects of seriously exceeding the standard of residues of agricultural and sideline products cannot be underestimated. Repeatedly causing acute poisoning and even death, the country has decided to stop the production of these four highly toxic pesticides by the end of 2005. Therefore, it is imminent to optimize the variety structure of China's pestici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N53/02C07C69/743
Inventor 唐炎森涂海兰沈行奂陈磊王怡敏
Owner SHANGHAI PESTICIDE RES INST
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