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Method for producing cloquintocet-mexyl

A technology for detoxifying quinoline and hydroxyquinoline, applied in botany equipment and methods, chemicals for biological control, biocides, etc., can solve the problem of high requirements for reaction temperature and pressure, incomplete esterification reaction, and long reaction time and other problems, to achieve the effect of mild reaction conditions, easy process control, and good product quality

Inactive Publication Date: 2013-07-10
新沂市永诚化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main defect of this operational route is: 1. in the reaction process, because the esterification reaction of chloroacetic acid and 2-heptanol is not complete, the reaction time is longer, and the yield is low, so it is not suitable for large-scale batch production; 2. .The requirements for reaction temperature and pressure are high, and the purification of intermediates is difficult, which in turn leads to the synthesis of detoxaquine with many impurities, low purity, and low yield, which affects product quality
[0005] The company once submitted a patent application of "A New Method for Synthesizing Jieduquine" with the patent application number 2010101516033 on April 21, 2010, but it has not been authorized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] After adding 5-chloro-8-hydroxyquinoline, solvent 1, and catalyst 1 in the chemical reaction kettle, start stirring, and the stirrer speed is 25 rpm. After stirring evenly, add solvent 2, catalyst 2, and the reaction is exothermic. Strictly monitor the temperature of the reaction solution in the reactor, and control the temperature in the reactor to be 110°C by sending steam or cold water to the interlayer of the reactor. After reacting for 0.9 hours, observe the solvent 2 refluxing in the reflux pipe of the reactor. When the refluxing solvent 2 is clear, the reaction ends, and the temperature in the kettle is lowered to 60°C by sending cold water into the interlayer of the reaction kettle, and the stirring is continued, and methyl chloroacetate is started to be added dropwise, and the molar ratio of the added amount is controlled as follows: 5-chloro- 8-Hydroxyquinoline: methyl chloroacetate: solvent 1: solvent 2: catalyst 1: catalyst 2=1:1:4:4:0.2:0.2, the reaction tem...

Embodiment 2

[0020] After adding 5-chloro-8-hydroxyquinoline, solvent 1, and catalyst 1 in the chemical reaction kettle, start stirring, and the stirrer speed is 30 rpm. After stirring evenly, add solvent 2, catalyst 2, and the reaction is exothermic. Strictly monitor the temperature of the reaction solution in the reactor, and control the temperature in the reactor to be 120°C by sending steam or cold water to the interlayer of the reactor. After reacting for 0.8 hours, observe the solvent 2 returned in the return pipe of the reactor. When the refluxing solvent 2 is clear, the reaction ends, and the temperature in the kettle is lowered to 65°C by sending cold water into the interlayer of the reaction kettle, and the stirring is continued, and methyl chloroacetate is started to be added dropwise, and the molar ratio of the added amount is controlled as: 5-chloro- 8-Hydroxyquinoline: methyl chloroacetate: solvent 1: solvent 2: catalyst 1: catalyst 2=1:1:4.5:3.5:0.2:0.2, the reaction temperat...

Embodiment 3

[0022]After adding 5-chloro-8-hydroxyquinoline, solvent 1, and catalyst 1 in the chemical reaction kettle, start stirring, and the stirrer speed is 35 rpm. After stirring evenly, add solvent 2, catalyst 2, and the reaction is exothermic. Strictly monitor the temperature of the reaction solution in the reactor, and control the temperature in the reactor to be 130°C by sending steam or cold water to the interlayer of the reactor. After reacting for 0.7 hours, observe the solvent 2 returned in the reflux pipe of the reactor. When the refluxing solvent 2 is clear, the reaction ends, and the temperature in the kettle is lowered to 70°C by sending cold water into the interlayer of the reaction kettle, and the stirring is continued, and methyl chloroacetate is started to be added dropwise, and the molar ratio of the added amount is controlled as follows: 5-chloro- 8-Hydroxyquinoline: methyl chloroacetate: solvent 1: solvent 2: catalyst 1: catalyst 2=1:1:5:3:0.2:0.2, the reaction tempe...

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PUM

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Abstract

The invention discloses a method for producing cloquintocet-mexyl, and belongs to the field of herbicides. By taking 5-chlorine-8-hydroxyquinoline, methyl chloroacetate, 2-heptanol, a solvent 1, a solvent 2, a solvent 3, a catalyst 1, a catalyst 2 and a catalyst 3 as raw materials, the method comprises the following steps: 1) synthesizing an intermediate 5-chlorine-8-quinoline oxygroup methyl acetate; and 2) synthesizing the cloquintocet-mexyl, thereby obtaining a final product. The method has the advantages that the general-purpose equipment is adopted; the process is simple; and the reaction condition is moderate. By utilizing the synthesizing method of ester exchange, the synthesized cloquintocet-mexyl is less in impurity, high in purity, high in yield and good in quality. The cloquintocet-mexyl is mainly utilized to be compounded with clodinafop-propargyl at a ratio of 1:4 so as to form the herbicide.

Description

technical field [0001] The invention belongs to the field of herbicides, and in particular relates to a method for producing acetoquine. Background technique [0002] Jieduquine, also known as Jieduquine, has a chemical name of 1-methylhexyl (5-chloro-8-quinolineoxy) acetate, a molecular weight of 335.8, and a molecular formula of C18H22ClNO3. The industrial appearance is a light yellow solid powder with a melting point of The temperature is 69.4°C, the density is 1.05 g / cm3, the solubility in water at 25°C is 0.54 mg / L, 190 mg / L in ethanol, 340 mg / L in acetone, and 360 mg / L in toluene. It is neutral and acidic Stable in the environment, easily hydrolyzed under alkaline conditions. The dosage form of jieduquine is emulsifiable concentrate or wettable powder, which is mainly used to improve the acceptance of plants to herbicides. Jieduquine is always combined with a herbicide when used, as a herbicide safener to control the annual grass in small grains; in use, Jieduquine i...

Claims

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Application Information

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IPC IPC(8): C07D215/28A01N43/42A01N43/40A01P13/00
Inventor 应冰如刘慧
Owner 新沂市永诚化工有限公司
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