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Process for synthesizing ryzalin by trichloromethyl carbonate method

A synthesis process and amisulfulazine technology, applied in the field of pesticide chemical industry, can solve problems such as serious pollution, and achieve the effects of improved process yield, mild reaction conditions and good product quality

Active Publication Date: 2009-07-08
江苏乐斯化学有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, during the ammonolysis reaction, the use of ammonia water will produce a large amount of orange-red production wastewater, causing serious pollution.

Method used

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  • Process for synthesizing ryzalin by trichloromethyl carbonate method

Examples

Experimental program
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Effect test

Embodiment 1

[0012] In a 250ml three-necked flask equipped with electric stirring, put 12g of 99.5% solid phosgene, then throw in 60ml of dichloroethane, start stirring, stir fully to dissolve it completely, and obtain a solid phosgene solution, which is then transferred to the dropping funnel middle. In addition, in a 500ml three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, put 36.9 g (100% off) of dry sodium 3,5-dinitro-4-dipropylaminobenzenesulfonate, dichloroethane 100ml, start stirring for 10min to dissolve the material, then add about 1.0g of DMF, control the temperature at about 15°C, and add the solid phosgene solution dropwise. After dropping, the reaction was continued to stir for 2 h at this temperature, and then heated to reflux for 1 h. Then cool to below 10°C, add 100ml of water, and pour in liquid ammonia under stirring. Control the ammonia flow rate and cooling water so that the temperature of the material does not exceed 50°C unt...

Embodiment 2

[0014] In Example 1, the inert solvent dichloroethane was changed to dichloromethane, and the consumption was the same; the remaining raw materials and operating conditions were unchanged. Then 32.1 g of orange-red dry powder was obtained, the content detected by HPLC was 98.15%, and the yield was 91.06% based on sodium 3,5-dinitro-4-dipropylaminobenzenesulfonate.

Embodiment 3

[0016] In Example 1, the inert solvent dichloroethane was changed to trichloromethane, and the consumption was the same; the remaining raw materials and operating conditions were unchanged. Then 31.8 g of orange-red dry matter was obtained, the content detected by HPLC was 98.24%, and the yield was 90.09% based on sodium 3,5-dinitro-4-dipropylaminobenzenesulfonate.

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Abstract

The invention relates to technology for synthesizing oryzalin by a trichloromethyl carbonic ether method, which relates to technology for synthesizing herbicide, namely the oryzalin. The technology is to take 3,5-binitro-4-di-n-propylamine benzene sulfonate as a raw material, use trichloromethyl carbonic ether to perform acyl chlorination in an inert solvent, and perform aminolysis to obtain crude oryzalin medicines. The innovation of the technology is to adopt the trichloromethyl carbonic ether instead of commonly used phosphorus oxychloride as an acyl chlorination agent, adopt dichloroethane to replace toluene, and finally use an ammonia liquid for direct aminolysis. The technology has the characteristics of cheap and easily obtained raw materials, safe, simple and convenient operation, high process yield, good product quality and small wastewater amount.

Description

Technical field: [0001] The invention relates to a method for synthesizing a pesticide herbicide, specifically a production process for preparing amisulfamelan by using 3,5-dinitro-4-dipropylaminobenzenesulfonate, and belongs to the field of pesticide chemical industry. Background technique: [0002] Oryzalin, commonly known as Oryzalin, has a chemical name of 3,5-dinitro-4-dipropylbenzenesulfonamide, and is the main species of dinitroaniline herbicides. There are two industrial production methods of amisulfameling, one is to use o-chloronitrobenzene as the starting raw material, and it is prepared by chlorosulfonation, dinitration, ammonolysis, and amination; the cost is caused by the high cost of raw materials and the large amount of chlorosulfonic acid Higher, acidic waste water and waste gas are more, and equipment corrosion is serious. The other one uses chlorobenzene as the starting material, and is prepared through sulfonation, nitration, salting out, amination, acyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/39C07C303/38A01P13/00
Inventor 陈呈新雷进海张捷龙
Owner 江苏乐斯化学有限公司
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