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Method for continuously preparing bentazone

A bentazon and flow rate control technology, applied in the direction of organic chemistry, can solve the problems of equipment corrosion, easily lead to material flushing, slow reaction speed, etc., and achieve the effects of high safety, improved production efficiency, and increased yield

Inactive Publication Date: 2020-06-12
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, route three has the following problems. The reaction process uses the raw material isopropylamine for the reaction. The boiling point of isopropylamine is low, only 33-34°C, and the exothermic heat in the sulfonylation reaction is severe, which easily leads to material flushing; secondly, chlorination-sulfonylation Phosphorus oxychloride is used as the chlorination reagent in the acylation process, which is easy to be volatile and hydrolyzed, which seriously corrodes the equipment; in the ring-closing reaction, the reaction speed is slow and the economic benefit is low

Method used

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  • Method for continuously preparing bentazone
  • Method for continuously preparing bentazone
  • Method for continuously preparing bentazone

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Such as figure 1 and figure 2 As shown, isopropylamine 22g and acid-binding agent triethylamine 145g are miscible with solvent dichloroethane 200g as material A, chlorosulfonic acid 38.2g as material B, methyl anthranilate 45g as material C, BTC53. 06 g and solvent dichloroethane 250g are miscible as material D, material A and material B are transported into tubular reactor R1 through infusion pump P1 and infusion pump P2 respectively, and the temperature of tubular reactor R1 is controlled by a water bath to 0°C. By setting the flow rate of the pump to control the residence time of the material in the tubular reactor R1 to 0.4min, the sulfonylation reaction is carried out in the tubular reactor R1 to generate isopropylamine sulfonic acid, and then the isopropylamine sulfonic acid is transported with the infusion pump P3 The material C is mixed, and the mixed material enters the tubular reactor R2 together with the material D delivered by the infusion pump P4. The tem...

Embodiment 2

[0033] Such as figure 1 and figure 2As shown, 24.66g of isopropylamine and 145g of acid-binding agent triethylamine are miscible with 200g of solvent dichloroethane as material A, 45.14g of chlorosulfonic acid as material B, 45g of methyl anthranilate as material C, BTC88 .43 g and solvent dichloroethane 250g are miscible as material D, material A and material B are transported into tubular reactor R1 through infusion pump P1 and infusion pump P2 respectively, and the temperature of tubular reactor R1 is controlled by a water bath to be 15°C , the residence time of the material in the tubular reactor R1 is controlled to be 1.0min by setting the pump flow rate, and the sulfonylation reaction is carried out in the tubular reactor R1 to generate isopropylamine sulfonic acid, and then the isopropylamine sulfonic acid is mixed with the infusion pump P3 The transported material C is mixed, and the mixed material enters the tubular reactor R2 together with the material D transporte...

Embodiment 3

[0035] like figure 1 and figure 2 As shown, 29.95g of isopropylamine and 145g of acid-binding agent triethylamine are miscible with 200g of solvent dichloroethane as material A, 55.56g of chlorosulfonic acid as material B, 45g of methyl anthranilate as material C, BTC123 .8 g and solvent dichloroethane 250g are miscible as material D, material A and material B are transported into tubular reactor R1 through infusion pump P1 and infusion pump P2 respectively, and the temperature of tubular reactor R1 is controlled by a water bath to be 30°C , by setting the pump flow rate to control the residence time of the material in the tubular reactor R1 to be 1.5min, the sulfonylation reaction is carried out in the tubular reactor R1 to generate isopropylamine sulfonic acid, and then the isopropylamine sulfonic acid is mixed with the infusion pump P3 The transported material C is mixed, and the mixed material enters the tubular reactor R2 together with the material D transported by the ...

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Abstract

The invention discloses a method for continuously preparing bentazone. The method comprises the following steps of: dissolving isopropylamine and an acid-binding agent in a solvent as a material A; with a methanol solution of sodium methoxide as a material F, feeding the material A and chlorosulfonic acid to a tubular reactor R1 for sulfonylation reaction; mixing the obtained isopropylamino sulfonic acid with methyl anthranilate, and then conveying the mixture and BTC to a tubular reactor R2 for chlorination-sulfonylation reaction; enabling the reaction liquid and the material F to enter a tubular reactor R3 for cyclization reaction, and adding inorganic acid at low temperature for acidification, so as to obtain a bentazone finished product. According to the method, BTC is adopted for chlorination-sulfonylation reaction, so that the problem that equipment is corroded by acid generated by volatilization and hydrolysis of phosphorus oxychloride is avoided, the whole process is continuousand controllable, the online quantity of raw materials is small, the safety is high, airtight, continuous and automatic production is easy to realize, the post-treatment is simple, and the method issuitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for continuously preparing bendazone. Background technique [0002] Bentazon, successfully developed by the German BASF company in 1966, is a herbicide with high efficiency, low toxicity, low residue, wide herbicidal spectrum, and strong selectivity. At present, bendazone is widely used in the world and has good application prospects and research value. [0003] There are mainly three kinds of bendazone synthetic routes reported in the literature: (1) methyl anthranilate route: first react with isopropylaminosulfonyl chloride and methyl anthranilate, and then use sodium methoxide ring closure to obtain bendazone (DE3428837), which was produced by this method in the early days. (2) Bright red acid anhydride route: bright red acid anhydride and isopropylamine react to obtain anthranilic acid isopropylamine, then in the presence of 2-picoline, carry out sulfonation with sulfur trioxide chlorosulfonic acid, then in trich...

Claims

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Application Information

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IPC IPC(8): C07D285/16
CPCC07D285/16
Inventor 余志群林金毅苏为科
Owner ZHEJIANG UNIV OF TECH
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