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Preparation method for 3-(2,2-dichloroethyenyl)-2,2-dimethylcyclopropanecarboxylic acid

A technology for chrysanthemic acid and chrysanthemic acid is applied in the field of preparation of trans-D-DV chrysanthemic acid, can solve the problems of high cost, complicated process, long production process of trans-D-DV chrysanthenic acid, etc., and achieves significant economic benefits and efficiency. The effect of social benefit

Active Publication Date: 2016-01-27
正泓(盘锦)精细化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a preparation method of trans-dextrorotary DV chrysanthemic acid, which is used to solve the problems of long production process, complex process and high cost of trans-dextrorotary DV chrysanthemic acid prepared by the existing split method

Method used

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  • Preparation method for 3-(2,2-dichloroethyenyl)-2,2-dimethylcyclopropanecarboxylic acid

Examples

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preparation example Construction

[0024] A kind of preparation method of trans-D-DV chrysanthemic acid provided by the invention comprises the following steps:

[0025] Step 1: Preparation of trans-swirling DV chrysanthemic acid solution, add 200g of trans-swirling DV chrysanthemic acid to 1000-2000g mother liquor under stirring, saponify with alkali such as ammonia water or NaOH aqueous solution, and adjust the pH value to 6.5 ~8.2, prepare the trans-swirl DV chrysanthemate solution;

[0026] Wherein, the trans-swirling DV chrysanthemic acid is a solid insoluble in water, and after adding an alkali such as ammonia water, the trans-swirling DV chrysanthemic acid is soluble in water to form a trans-swirling DV chrysanthemic acid salt solution.

[0027] Step 2: Preparation of an aqueous solution of the resolving agent, dissolving 90-110 g of the resolving agent in water under stirring and adjusting the pH value to 2-5 by adding acid to prepare an aqueous solution of the resolving agent.

[0028] Step 3: Splitti...

Embodiment

[0047] Add 1200g of water to a 2000ml three-necked bottle, put in 200g of trans-swirl DV chrysanthemic acid, start stirring, add ammonia dropwise to adjust the pH value to 7.2;

[0048] Add 100g of resolving agent to a 1000ml three-necked bottle, add 350g of water, start stirring to dissolve the resolving agent into a resolving agent solution, add hydrochloric acid to adjust the pH value to 3.6.

[0049]Add the resolving agent solution dropwise to the above-mentioned 2000ml three-necked flask under stirring, the operating temperature is 35°C, the dropwise addition time is 85 minutes, after the dropwise addition, keep warm for 20 minutes, add 300g of toluene, and form solid particles after 18 minutes. Stand to separate the water phase A10, add 500 g of water to wash the solid particles, and separate the water phase B10. Put the water phase A10 and water phase B10 in another three-necked bottle, acidify and adjust the pH value to 2.5 to obtain trans-DV chrysanthemic acid and wat...

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Abstract

The invention provides a preparation method for 3-(2,2-dichloroethyenyl)-2,2-dimethylcyclopropanecarboxylic acid. The preparation method comprises the following steps: adding 200 g of trans-(+ / -)-DV-chrysanthemic acid into 1000 to 2000 g of mother liquor under stirring and adjusting a pH value to 6.5 to 8.2 by using alkali so as to produce a trans-(+ / -)-DV-chrysanthemate solution; dissolving 90 to 110 g of a resolving agent in water under stirring and adjusting a pH value to 2 to 5 by using acid so as to obtain an aqueous solution of the resolving agent; adding the aqueous solution of the resolving agent into the trans-(+ / -)-DV-chrysanthemate solution drop by drop within 1 to 3 h under stirring to produce a solution including solid double salt; adding 200 to 400 g of a separating agent into the solution including the solid double salt under stirring and carrying out stirring to separate a solid double salt particle and a water phase; and adding acid under stirring to adjust the pH value of separated water phase liquid to 2 to 4 so as to form a solid and an aqueous solution, wherein the solid is 3-(2,2-dichloroethyenyl)-2,2-dimethylcyclopropanecarboxylic acid. The preparation method provided by the invention overcomes the problems of long production flow, complex process and high cost in conventional resolution methods for preparation of 3-(2,2-dichloroethyenyl)-2,2-dimethylcyclopropanecarboxylic acid.

Description

technical field [0001] The invention relates to a preparation method of trans-D-DV chrysanthemic acid (also known as DV chrysanthemic acid), that is, the preparation process is realized by splitting. Background technique [0002] Trans-D-DV chrysanthemic acid is an important intermediate in the production of pyrethroid insecticide transfluthrin chiral pesticide. Due to the increasing calls for environmental protection, the improvement of pesticide management regulations, and the constraints of various factors such as market and efficiency, the use of a single isomer to develop high-efficiency, low-toxicity, low-cost, and non-harmful chiral pesticides has become the development of pesticides. How to obtain chiral pesticide intermediates is the key to the synthesis of chiral pesticides, and also determines the production process and cost of pesticide products. [0003] As an intermediate, trans-dextrorotatory DV chrysanthemic acid is a domestic blank product, and only Bayer (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C61/40C07C51/42C07C51/41C07C51/02C07C51/487C07B57/00
Inventor 黄春宝
Owner 正泓(盘锦)精细化工科技有限公司
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