Production method of bentazone technical

A production method and a technology of bentazone, applied in the field of pesticide compounds, can solve the problems of high production cost, dust pollution, low purity and the like, and achieve the effects of high production efficiency, low environmental pollution and simple operation

Inactive Publication Date: 2017-12-08
江苏绿叶农化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has the problems of high production cost, complex production method, harsh production conditions, a large amount of saline waste water pollution, serious dust pollution, and low yield and low purity of the product obtained in the production process.

Method used

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  • Production method of bentazone technical

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of production method of the former medicine of bentazone that the present invention proposes, comprises the following steps:

[0018] S1. Preparation of o-amino-N-isopropylbenzamide: Dissolve isatoic anhydride in dichloroethane, add isopropylamine dropwise while heating up, heat up to 48°C, keep warm for 0.5h, and then use saturated carbonic acid Wash with sodium to remove ethylene dichloride to obtain light yellow o-amino-N-isopropylbenzamide solution, wherein the mass ratio of isatoic anhydride, ethylene dichloride and isopropylamine is 2:2:1;

[0019] S2, preparation of bentazone technical substance: add α-picoline and ethylene dichloride to the o-amino-N-isopropylbenzamide obtained in step S1 and mix, add sulfur trioxide dropwise to generate translucent milky white After stirring at room temperature for 0.4h, add the preheated amide dichloroethane, stir until the crystallized amide pyridine sulfur trioxide double salt is precipitated, add the catalyst, then d...

Embodiment 2

[0021] A kind of production method of the former medicine of bentazone that the present invention proposes, comprises the following steps:

[0022] S1. Preparation of o-amino-N-isopropylbenzamide: Dissolve isatoic anhydride in dichloroethane, add isopropylamine dropwise while heating up, heat up to 60°C, keep warm for 0.8h, and then use saturated carbonic acid Washing with sodium to remove ethylene dichloride gives light yellow o-amino-N-isopropylbenzamide solution, wherein the mass ratio of isatoic anhydride, ethylene dichloride and isopropylamine is 3.5:2.6:1.8;

[0023] S2, preparation of bentazone technical substance: add α-picoline and ethylene dichloride to the o-amino-N-isopropylbenzamide obtained in step S1 and mix, add sulfur trioxide dropwise to generate translucent milky white After stirring at room temperature for 0.7h, add the preheated amide dichloroethane, stir until the crystallized amide pyridine sulfur trioxide double salt is precipitated, add the catalyst, t...

Embodiment 3

[0025] A kind of production method of the former medicine of bentazone that the present invention proposes, comprises the following steps:

[0026] S1. Preparation of o-amino-N-isopropylbenzamide: Dissolve isatoic anhydride in dichloroethane, add isopropylamine dropwise while heating up, heat up to 52°C, keep warm for 0.6h, and then use saturated carbonic acid Washing with sodium to remove ethylene dichloride gives light yellow o-amino-N-isopropylbenzamide solution, wherein the mass ratio of isatoic anhydride, ethylene dichloride and isopropylamine is 2.5:2.2:1.2;

[0027] S2, preparation of bentazone technical substance: add α-picoline and ethylene dichloride to the o-amino-N-isopropylbenzamide obtained in step S1 and mix, add sulfur trioxide dropwise to generate translucent milky white After stirring at room temperature for 0.5h, add the preheated amide dichloroethane, stir until the crystalline amide pyridine sulfur trioxide double salt is precipitated, add the catalyst, th...

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PUM

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Abstract

The invention discloses a production method of bentazone technical. The production method comprises the following steps: enabling isatoic anhydride, dichloroethane and isopropylamine to react; washing with saturated sodium carbonate to remove the dichloroethane and obtain an o-amino-N-isopropyl benzamide solution; adding alpha-methylpyridine and the dichloroethane into the o-amino-N-isopropyl benzamide solution and mixing; dropwise adding sulfur trioxide, amide dichloroethane, a catalyst and a phosphorus oxychloride solution, and heating till reflux; cooling to room temperature; performing hydrolysis, alkaline washing and water washing; extracting with dilute alkaline liquid; layering to obtain bentazone sodium salt; acidifying and filtering to obtain a light yellow solid; drying to obtain the bentazone technical. According to the production method of the bentazone technical disclosed by the invention, a few steps are adopted, the operation is simple, alkali or acid is not adopted in the production process to ensure little environmental pollution, the production efficiency is high, the yield of the obtained bentazone technical can reach 90% or above, the purity of the bentazone technical is as high as 98.5% or above, and the production method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of pesticide compounds, in particular to a production method of bentazone technical. Background technique [0002] Benazone is an important post-emergence herbicide, its chemical name is 3-isopropyl-(1H)-benzo-2,1,3-thiadiazin-4-one-2,2-dioxide It was originally successfully developed by the German BASF company and widely used around the world. It is a selective contact-killing post-emergence herbicide, which is used to treat the stems and leaves of weeds at the seedling stage. For crops such as peanuts and wheat, it can control broad-leaved weeds and sedge weeds, but is ineffective against gramineous weeds. In the prior art, the preparation process of bentazone technical mostly adopts methods such as alkaline extraction, acidification, water washing of bentazone dichloroethane solution after synthetic washing, and alkaline extraction, acidification, extraction and concentration. The above method has the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/16
CPCC07D285/16
Inventor 陈标
Owner 江苏绿叶农化有限公司
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