A kind of preparation method of trans DV chrysanthemic 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: 2017-10-31
正泓(盘锦)精细化工科技有限公司
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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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  • A kind of preparation method of trans DV chrysanthemic acid

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preparation example Construction

[0024] The invention provides a preparation method of trans-D-DV chrysanthemum acid, which comprises the following steps:

[0025] Step 1: Preparation of trans-mixed DV chrysanthemum acid salt solution. Under stirring, add 200g of trans-mixed DV chrysanthemum acid to 1000~2000g mother liquor, saponify with ammonia or NaOH aqueous solution, etc., and adjust the pH to 6.5 ~8.2, to prepare a trans-mixed DV chrysanthemum salt solution;

[0026] Among them, the trans-mixed DV chrysanthemum acid is a solid insoluble in water. After adding ammonia and other alkalis, the trans-mixed DV chrysanthemum acid salt is soluble in water to produce a trans-mixed DV chrysanthemum acid salt solution.

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

[0028] Step 3: Resolve, add dropwise the resolving agent aqueous solution pre...

Embodiment

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

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

[0049] Under stirring, the resolving agent solution was added dropwise to the above-mentioned 2000ml three-necked flask, the operating temperature was 35°C, the dropping time was 85 minutes, and the temperature was kept for 20 minutes after the dropping. 300g of toluene was added, and solid particles were formed after 18 minutes. The water phase A10 was separated by standing, and 500 g of water was added to wash the solid particles, and the water phase B10 was separated. Put the water phase A10 and water phase B10 in another three-necked bottle, acidify and adjust the pH to 2.5 to ...

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Abstract

The present invention proposes a preparation method of trans dextrorotatory DV chrysanthemic acid, comprising: adding 200 g of trans dextrorotatory DV chrysanthemic acid into 1000-2000 g of mother liquor under stirring, adjusting the pH value to 6.5-8.2 with alkali, Generate a trans-swirling DV chrysanthemum salt solution; dissolve 90-110g of the resolving agent in water under stirring, add acid to adjust the pH value to 2-5, and obtain an aqueous solution of the resolving agent; dissolve the aqueous solution of the resolving agent under stirring Add dropwise to the trans-swirling DV chrysanthemum salt solution for 1 to 3 hours to generate a solution containing solid double salt; add 200 to 400 g of separating agent to the solution containing solid double salt under stirring, and stir so that Separating the solid double salt particles and the water phase; adding acid under stirring to adjust the pH value of the separated water phase to 2-4 to form a solid and an aqueous solution, and the solid is trans-DV chrysanthemic acid. The invention solves the problems of long production process, complex process and high cost for preparing trans-DV chrysanthemic acid by the existing resolution method.

Description

Technical field [0001] The invention relates to a preparation method of trans-D-DV chrysanthemum acid (also known as DV chrysanthemum acid), that is, the preparation process is realized through resolution. Background technique [0002] Trans-dextrorotatory DV chrysanthemum acid is an important intermediate for the production of pyrethroid insecticide tetrafluthrin chiral pesticide. Due to the increasing demand for environmental protection, the improvement of pesticide management regulations, and the constraints of factors such as market and efficiency, the use of single isomers to develop high-efficiency, low-toxicity, low-cost, and non-toxic chiral pesticides has become the development of pesticides. Trends, and 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-D-DV chrysanthemum acid is a domestic blank product. Only Bayer in ...

Claims

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Application Information

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Patent Type & Authority Patents(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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