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New process for preparing tribenuron-methyl by using one-pot method

A technology for trisulfuron-methyl and a new process is applied to the field of a new process for preparing trisulfuron-methyl by a one-pot method, which can solve the problems of increasing triphosgene leakage, high consumption, difficult quantitative reaction, etc. Danger, reduce energy waste, simplify the effect of the reaction device

Inactive Publication Date: 2012-03-28
ANHUI FENGLE AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The oxalyl chloride method has the problems of large consumption, high cost and difficulty in popularization
The phosgene method has disadvantages such as highly toxic phosgene, inconvenient storage and transportation, difficult quantitative reaction, and long reaction time.
Solid phosgene method The method reported in the literature so far is to dissolve solid phosgene in a solvent and drop it into the reaction solution. Therefore, this method needs to increase the dissolution kettle and the dropping device, thereby increasing the leakage of three phosgenes. danger, and the reaction time is longer; in addition, different solvents are used in the subsequent reaction, so different containers and pipelines need to be added, and the reaction is carried out under reflux, which consumes a lot of energy

Method used

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  • New process for preparing tribenuron-methyl by using one-pot method

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Experimental program
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Effect test

Embodiment 1

[0006] Embodiment 1: a new preparation process of tribenuron-methyl, the process is first reacted with methyl o-formate benzenesulfonamide and solid phosgene, and the reaction product continues to react with methyl triazine to prepare tribenuron-methyl, the reaction formula is as follows:

[0007]

[0008] In a 500 ml four-neck flask equipped with a thermometer, a stirrer and a condenser tube, add 0.1 mol of methyl o-formate benzenesulfonamide, add 0.04 mol of solid phosgene, 0.06 mol of n-butyl isocyanate, and xylene 250 milliliters, heat up to reflux after stirring evenly, and after stirring for 3 hours under reflux, steam the catalyst and solvent under reduced pressure (for the next previous step reaction to apply directly), add 250 milliliters of fresh xylene solvent, add 0.1mol methyltriazine, the temperature of the reaction mixture solution was raised to 70° C., and the stirring was continued for 2 hours. After the reaction was finished, the solvent was precipitated u...

Embodiment 2

[0009] Embodiment two: in the 500 milliliter four-neck flasks that thermometer, stirrer and condensing pipe are equipped with, add the methyl o-formate benzene sulfonamide of 0.1mol, add the solid phosgene of 0.04mol, and the catalyst of reclaiming and 250 milliliters of solvents After stirring evenly, it was heated to reflux, and after stirring for 3 hours under reflux, the catalyst and solvent were evaporated under reduced pressure (continuing to apply mechanically next time), and 250 milliliters of xylene solvent was added, and 0.1mol of methyl triazine was added. , the temperature of the reaction mixed solution was raised to 70° C., and the stirring was continued for 2 hours. After the reaction, desolvation under reduced pressure (the solvent will be used next time), and post-treatment, drying to obtain 31.7 grams of product, the yield is 80.2% based on methyl o-formate benzenesulfonamide.

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Abstract

The invention provides a new process for preparing tribenuron-methyl. The process comprises the following steps of: performing first reaction in a solvent with a catalyst by using methyl o-sulphamoylbenzoate and solid phosgene, and continuously performing second reaction on the reaction product and methyl triazine to generate the tribenuron-methyl. The process is characterized in that: a one-pot method and a single dimethyl benzene solvent are adopted. By the process, the reaction device is simplified, the reaction time is shortened, the consumption of energy is reduced, and the total yield of the product reaches over 80 percent.

Description

technical field [0001] The invention belongs to the technical field of pesticides, and in particular relates to a new process for preparing tribenuron-methyl in one pot. Background technique [0002] Tribenuron-methyl is a sulfonylurea herbicide with high herbicidal activity, safety to crops and environmental friendliness. Its production method generally adopts the isocyanate route, and methyl o-formate benzenesulfonamide and oxalyl chloride react to obtain 2-methyl formate-3-benzenesulfonyl isocyanate or by methyl o-formate benzenesulfonamide and phosgene or triphosgene (solid phosgene gas) reaction to obtain 2-methyl formate-3-benzenesulfonyl isocyanate; the generated 2-methyl formate-3-benzenesulfonyl isocyanate reacts with methyl triazine to generate tribenuron. The oxalyl chloride method has the problems of large consumption, high cost and difficulty in popularization. The phosgene method has disadvantages such as highly toxic phosgene, inconvenient storage and transp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/16
Inventor 周康伦金劲松赵国平林昌志施亦敏凌朵朵陈克付
Owner ANHUI FENGLE AGROCHEM
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