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Nicosulfuron water-phase method synthesis process

A nicosulfuron-methyl and synthesis process technology, applied in the field of pesticides, can solve the problems of complex process, poor product quality and the like, and achieve the effects of low reaction temperature, good quality and sufficient reaction

Active Publication Date: 2021-04-13
HANDAN RUITIAN PESTICIDES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a nicosulfuron-methyl aqueous phase synthesis process, which solves the problems of complex processes and poor product quality in the related art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 301.68g of 2-ethoxycarbonylaminosulfonyl-N,N-dimethylnicotinamide, 155.64g of 2-amino-4,6-dimethoxypyrimidine, and 5.25g of tetrabutylammonium bromide into the reaction kettle , 0.3g[(C 4 h 9 ) 4 N] 3 PMo 12 o 40 , 0.6g pareth-12, 603.93g of acetonitrile aqueous solution with acetonitrile mass content of 50%, the temperature is controlled between 60-100°C, and the reaction is about 7 hours; centrifuged, dried and dried to obtain nicosulfuron-methyl 398.14 g, yield 96.89%, purity 98.81%.

Embodiment 2

[0023] Add 301.31g of 2-ethoxycarbonylaminosulfonyl-N,N-dimethylnicotinamide, 160.21g of 2-amino-4,6-dimethoxypyrimidine, and 7.1g of tetrabutylammonium bromide into the reaction kettle , 0.7g[(C 4 h 9 ) 4 N] 2 HPMo 12 o 40 , 1.39g of pareth-12, 750.13g of acetonitrile aqueous solution with acetonitrile mass content of 55%, the temperature was controlled between 60-100°C, and the reaction was carried out for about 6 hours; centrifuged, dried and dried to obtain nicosulfuron-methyl 398.58 g, yield 97.12%, purity 98.96%.

Embodiment 3

[0025] Add 301.57g of 2-ethoxycarbonylaminosulfonyl-N,N-dimethylnicotinamide, 170.65g of 2-amino-4,6-dimethoxypyrimidine, and 11.59g of tetrabutylphosphine bromide into the reaction kettle , 1.12g[(C 4 h 9 ) 4 N]H 2 PMo 12 o 40 , 2.31g of pareth-12, 900.64g of acetonitrile aqueous solution with a mass content of 60% in acetonitrile, controlled at a temperature between 60 and 100°C, and reacted for about 5 hours; centrifuged, dried, and obtained nicosulfuron-methyl 398.64 g, yield 97.13%, purity 99.01%.

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Abstract

The present invention relates to the technical field of pesticides, and provides a nicosulfuron water-phase method synthesis process, which comprises: S1, material feeding: adding 2-ethoxycarbonyl amino sulfonyl-N, N-dimethyl nicotinamide, 2-amino-4, 6-dimethoxypyrimidine, a phase transfer catalyst and a solvent to a reaction kettle, and starting stirring; S2, reacting at the temperature of 60-100 DEG C for 5-7 hours; and S3, discharging: centrifuging and drying to obtain the nicosulfuron. Through the technical scheme, the problems of complex process and poor product quality in the prior art are solved.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a synthesis process of nicosulfuron-methyl in an aqueous phase method. Background technique [0002] Nicosulfuron (trade name Yu Nongle) is a new generation of broad-spectrum, high-efficiency, low-toxicity, low-residue sulfonylurea herbicide, and it is one of the best herbicide varieties for corn fields so far. It mainly controls weeds by inhibiting acetolactase, and is an inhibitor of side chain amino acid synthesis. Applied after germination in cornfields, it can control annual and perennial grass weeds and some broad-leaved weeds. It degrades rapidly in the soil and has no effect on the next crops. [0003] The existing technology that adopts urethane and aminopyrimidine reaction to make nicosulfuron is to produce under the condition of toluene as solvent, and the toluene limit is refluxed and dehydrated, and reacts, but because the early stage reaction temperature is high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12B01J27/19B01J31/02B01J31/06
CPCC07D401/12B01J31/068B01J31/0239B01J31/0268B01J27/19B01J35/19Y02P20/584
Inventor 王学铭王鹏飞马立香张艳敏
Owner HANDAN RUITIAN PESTICIDES CO LTD
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