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Method for preparing fenpropathrin

A technology of fenpropathrin and fenpropathrin, which is applied in the field of preparation of pyrethroids, can solve the problems of not getting fenpropathrin, etc., and achieve the effects of simple separation, high yield and reduced production cost

Inactive Publication Date: 2010-05-19
JIANGSU HUANGMA AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But applicant can not obtain fenpropathrin according to the method of this patent

Method used

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  • Method for preparing fenpropathrin

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Embodiment 1

[0017] The method for preparing fenpropathrin of the present embodiment has the following steps:

[0018] ① Prepare a mixed solution. In 2000L reactor, add 200kg purity and be 99% ether aldehyde (1kmol), 235.2kg concentration be 25% sodium cyanide aqueous solution (1.2kmol), 200kg cyclohexane solvent and 300g 4,4-dimethylamino pyridine and stirred to obtain a mixed solution.

[0019] ② Prepare the crude product containing fenpropathrin. By formocyanyl chloride, step 1. ether aldehyde and sodium cyanide in the mixed solution as reactant, by step 1. 4,4-dimethylaminopyridine in the mixed solution as catalyst, by step 1. cyclohexane in the mixed solution As a solvent, carry out the chemical reaction of generating fenpropathrin as follows: at a temperature of 15° C., 164 kg of 98% formcyanoyl chloride (1 kmol) is added dropwise to the above-mentioned mixed solution within 5 h from the overhead tank, and then in 30 The reaction was carried out at ℃ for 4 hours, and the crude pro...

Embodiment 2~ Embodiment 7

[0022] Each embodiment is basically the same as Embodiment 1, and the differences are shown in Table 1.

[0023] Table 1

[0024]

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PUM

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Abstract

The invention discloses a method for preparing fenpropathrin. The method comprises the following: (1) a step of preparing mixed solution, which is to mix ether aldehyde, sodium cyanide aqueous solution, organic solvent and aminopyridine or derivatives thereof serving as a phase transfer catalyst so as to obtain the mixed solution; (2) a step of preparing a fenpropathrin-containing crude product, which is to add methyl cyanide acyl chloride dropwise to the mixed solution obtained in a step (1) at 10 to 20 DEG C, perform thermal insulation reaction for 3 to 6 hours at 20 to 40 DEG C and obtain the fenpropathrin-containing crude product; and (3) a step of refining, which is to layer the fenpropathrin-containing crude product obtained in a step (2), remove cyanide-containing wastewater layers, use water to wash oil layers to be neutral, remove the organic solvent and obtain fenpropathrin crude oil. The method can obtain the fenpropathrin crude oil with high purity, excellent color and high yield, is simple in separation, needs no recrystallization, avoids the production of waste mother liquor, and reduces production cost.

Description

technical field [0001] The invention relates to a method for preparing pyrethroids, in particular to a method for preparing fenpropathrin. Background technique [0002] Fenpropathrin is a pyrethroid pesticide whose chemical name is methyl α-cyano-3-phenoxyphenyl-2,2,3,3-tetramethylcyclopropanecarboxylate. It can be used not only as a single insecticide, but also in combination with other types of insecticides and acaricides. Its main features are high efficiency, low pollution, low drug resistance, and low cost of use. [0003] Chinese patent document CN1041721C discloses a kind of preparation of fenpropathrin from tetramethylcyclopropane carboxylic acid through cyanohydrin method. Since this method first cyanates ether aldehyde (also known as m-phenoxybenzaldehyde or 3-phenoxybenzaldehyde) to generate cyanohydrin compounds, the highly toxic substance hydrocyanic acid will be produced in this process, which has potential safety hazards. . Moreover, the cyanohydrin compou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/39C07C253/14
Inventor 宦志东
Owner JIANGSU HUANGMA AGROCHEM
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