Preparation technology of DV-chrysanthemyl chloride with cis-trans ratio of 80:20-25:75

A preparation process, the technology of chrysanthemum acid chloride, which is applied in the field of preparation process of DV-chrysanthemum acid chloride with a cis-trans ratio of 80:20-25:75, can solve the problems of complex process, low product yield and high cost of raw materials

Inactive Publication Date: 2012-10-10
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

High cost of raw materials, com...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 340 grams of tert-butanol to a 1000-milliliter four-neck flask equipped with a stirring and thermometer, and slowly add 29.25 grams (0.75 moles) of sodium amide under ice-water cooling to control the reaction temperature at 30-40°C. The reaction was stirred at room temperature for 0.5 hours to obtain a sodium tert-butoxide solution in tert-butanol. Then add 48 grams of DMF and 62 grams of n-hexane, stir evenly and then cool down, cool the reaction solution below -5°C, add 191 grams (0.6 mol) of tetrachloroester with a content of 93% dropwise in 1-1.5 hours, in - Insulate and react at 5°C for 3 hours, then raise the temperature and reflux for 1 hour, sample and analyze, after the reaction is completed, distill the solvent to 100°C under negative pressure to obtain trichloride, content: 93%.

[0013] Add 280 grams of 30% liquid caustic soda (2.1 moles), 60 grams of water, 4 grams of tetrabutylammonium bromide, and 1 gram of cetyltrimethylammonium bromide in the obtain...

Embodiment 2

[0017] Replace the tetrabutylammonium bromide in example 1 with the same amount of benzyltriethylammonium chloride, all the other through the same process conditions and operating method, obtain 108 grams of permethrin intermediates and 112 grams of product DV-chrysanthemum Acid chloride, content: 98.5%, total yield (calculated as tetrachloroester): 82.05%, cis-trans ratio: 80:20.

Embodiment 3

[0019] Replace 1 gram of hexadecyltrimethylammonium bromide in example 1 with 0.5 gram of sodium lauryl polyoxyethylene ether sulfate (EO number is 3), all the other through the same process conditions and operating method, obtain 107 grams Permethrin intermediate and 111 grams of product DV-chrysanthemum acid chloride, content: 98.3%, total yield (calculated as tetrachloride): 81.3%, cis-trans ratio: 81:19.

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Abstract

The invention discloses a preparation technology of DV-chrysanthemyl chloride with a cis-trans ratio of 80:20-25:75, characterized by using tetrachloroate or trichloroate to prepare DV-chrysanthemic acid with different cis-trans ratios, then directly using the DV-chrysanthemic acid with different cis-trans ratios in the following reaction to prepare DV-chrysanthemyl chloride, wherein the content of the obtained DV-chrysanthemyl chloride is no less than 98%. In the process of using the technology to prepare the DV-chrysanthemic acid with different cis-trans ratios from tetrachloroate or trichloroate, cheap sodium hydroxide solution is utilized to replace sodium methoxide, the intermediate products have no need of refining method and can be directly used in the following reaction to prepare DV-chrysanthemyl chloride, and the content of the obtained DV-chrysanthemyl chloride is no less than 98%.

Description

Technical field [0001] The main task of the present invention is to provide a preparation process of DV-chrysanthemum chrysanthemum with a smooth ratio of 80: 20-25: 75, which are specifically prepared for low dv-chrysanthemum chrysanthemum and high-orchy DV-chrysanthemum chlorine, and then mixed up smoothly.The preparation process of DV-chrysanthemum chloride with 80: 20-25: 75. Background technique [0002] The traditional DV-chrysanthemum chlorine preparation process, when preparing DV-chrysanthexic acid by tetrachloride or trichloride, needs to be carried out by sodium sodium molten chloride and performed in methanol solvents.Intermediate, distilled recycling solvent.High cost of raw materials, complex craftsmanship, and low product revenue. Invention content [0003] The main task of the present invention is to provide a preparation process of DV-chrysanthemum chrysanthemum with a smooth ratio of 80: 20-25: 75. Specifically, a smooth ratio with a capable content of ≥98%is 8...

Claims

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Application Information

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IPC IPC(8): C07C61/40C07C51/60
Inventor 谭建平周甦谭金宝
Owner NANTONG TENDENCI CHEM
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