Method for synthesizing clethodim

A synthesis method and technology of clethodim, applied in the fields of botanical equipment and methods, herbicides and algicides, chemicals for biological control, etc., can solve the problem of high energy consumption, unstable clethodim, reaction temperature Advanced problems, to achieve the effect of preventing decomposition

Inactive Publication Date: 2009-11-11
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] (±)-2-[(E)-3-Chloroallyloxyimino]propyl-5-[2-(ethylthio)propyl]-3-hydroxycyclohex-2-enone is an agricultural The general name of the herbicide clethodim, the existing current reports use petroleum ether as a solvent to condense glycerone and allyloxyamine to prepare clethodim. No...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0010] Put 600 grams of petroleum ether, 50 grams of glycerone, and 1.5 grams of nitrogen-methylpyrrolidinone into a 1000ml three-neck flask, stir for 30 minutes, keep the temperature at 15-20°C with a water bath, and add allyloxyamine 20 g, keep the temperature at 25-20°C, react for 4 hours, detect that the content of allyloxyamine is less than 0.5%, the reaction is completed, then wash with acid water, and at 70°C, use negative pressure distillation to remove the aqueous solvent to obtain clexa Ketone, the yield is about 97%, and the content is 95%.

example 2

[0012] Put 600 grams of petroleum ether, 50 grams of glycerone, and 2.5 grams of nitrogen-methylpyrrolidinone into a 1000ml three-neck flask, stir for 30 minutes, keep the temperature at 15-20°C with a water bath, and add allyloxyamine 20 g, keep the temperature at 25-20°C, react for 4 hours, detect that the content of allyloxyamine is less than 0.5%, the reaction is completed, then wash with acid water, and at 70°C, use negative pressure distillation to remove the aqueous solvent to obtain clexa Ketone, the yield is about 97%, and the content is 94%.

example 3

[0013] Example three (comparative test):

[0014] Put 600 grams of petroleum ether and 50 grams of acetrione into a 1000ml three-necked flask, stir for 30 minutes, keep the temperature at 55-60°C, add 20 grams of allyloxyamine, keep the temperature at 55-60°C, and react 4 hours, the detection of allyloxyamine content is less than 0.5%, the reaction is over, and then washed with acid water, at 80 ° C, with negative pressure distillation, the water-containing solvent is removed, and clethodim is obtained. The yield is about 87%, and the content is 90%. .

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PUM

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Abstract

The invention relates to a method for synthesizing clethodim, in particular to a process for synthesizing an agricultural herbicide clethodim, namely (+/-)-2-[(E)-3-chloro-allyloxyimino]propyl-5-[2-(ethylthio)propyl]-3-hydroxy-cyclohexyl-2-keten. The method uses petroleum ether as a solvent and a ketone complex as a stabilizing agent to perform condensation reaction on propyl-triketone and allyl amine oxide to prepare the clethodim. Under the condition that the ketone complex serves as the stabilizing agent, the method can perform the condensation reaction at a low temperature by using the petroleum ether as the solvent, and prevent the clethodim product obtained through the reaction from being decomposed due to a high temperature to cause yield declination and content to decrease, thus the yield of the method can reach about 97 percent and the content reaches 94 percent.

Description

technical field [0001] The present invention relates to the agricultural herbicide clethodim, namely (±)-2-[(E)-3-chloroallyloxyimino]propyl-5-[2-(ethylthio)propyl]-3 -Synthetic process of hydroxycyclohex-2-enone. Background technique [0002] (±)-2-[(E)-3-Chloroallyloxyimino]propyl-5-[2-(ethylthio)propyl]-3-hydroxycyclohex-2-enone is an agricultural The general name of the herbicide clethodim, the existing current reports use petroleum ether as a solvent to condense glycerone and allyloxyamine to prepare clethodim. Not only the reaction temperature is high, but the production process consumes a lot of energy. Moreover, the yield is only about 86%, and the content is only 90%, which is not conducive to economical industrial production. In addition, the produced clethodim is extremely unstable at high temperature. Contents of the invention [0003] The object of the present invention is to invent a kind of synthetic method that improves reaction yield, increases the conte...

Claims

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Application Information

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IPC IPC(8): C07C323/47C07C319/20A01N41/12A01P13/00
Inventor 于国权俞玮吉志扬王建荣
Owner JIANGSU CHANGQING AGROCHEMICAL CO LTD
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