Method for manufacturing rich reverse type first chrysanthemic acid
A manufacturing method and technology of chrysanthemic acid, which is applied in the field of producing the first trans-rich chrysanthemic acid by melting crystallization method, can solve problems such as differences in insecticidal efficacy, and achieve the effects of low production cost, high yield and clean process
Active Publication Date: 2009-12-30
DALIAN CHEMPHY CHEM
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Problems solved by technology
As the acid moiety composition of pyrethroid pesticides, different isomers of the first chrysanthemic acid showed significant differences in their insecticidal efficacy
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[0022] Accurately weigh the first racemic (±) chrysanthemic acid, melt it completely at 60°C, stir and crystallize slowly at the corresponding crystallization temperature for 2 to 7 hours, and keep warm and filter, then heat up the jacket of the filter tank to make the crystal sweat, and put it while it is hot The liquid is extruded, the temperature is lowered and the crystal is transferred to obtain the first chrysanthemic acid rich in trans with a high cis-to-trans ratio, and the filtrate can be further melted and crystallized.
[0023]
[0024]
[0025]
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The invention provides a method for manufacturing a rich reverse type first chrysanthemic acid. The method is characterized by comprising the following steps: using a racemization (+ / -) first chrysanthemic acid with a purity of 93-99 percent and a forward inverse ratio between 3 / 97 and 20 / 80 as the material; crystallizing by means of melt crystallization at a temperature of 39.7-51 DEG C to obtain a rich reverse type first chrysanthemic acid with a forward inverse ratio of 1.5 / 98.5-9 / 91; and sweating, filtering and crystallizing the rich reverse type first chrysanthemic acid to obtain the rich reverse type first chrysanthemic acid with high purity, wherein the sweating temperature is 1-3 DEG C higher than the crystallizing temperature.
Description
technical field [0001] The present invention relates to rich trans-first chrysanthemic acid, and in particular provides a technology for producing rich trans-first chrysanthemic acid by melt crystallization. Background technique [0002] The first chrysanthemic acid (also known as chrysanthemic acid, English name Chrysanthemic acid) is an important intermediate compound composed of acid moieties in the synthesis of pyrethroid pesticides. The first chrysanthemic acid, namely 2,2-dimethyl-3-3(2-methyl-1-propenyl)cyclopropanecarboxylic acid, is shown in the following formula [0003] [0004] Because there are two chiral carbon atoms on its cyclopropane ring, it has two configurations of R (+) and S (-), and two isomers of cis and trans, and there are four isomers in total. As the acid moiety composition of pyrethroid pesticides, different isomers of the first chrysanthemic acid show significant differences in their insecticidal efficacy. For the cis and trans structures, ...
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Login to View More IPC IPC(8): C07C61/37C07C51/353C07C51/43
Inventor 邓东升徐海珍王明广尹宁宁
Owner DALIAN CHEMPHY CHEM
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