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Preparation method of high-purity profenofos

A profenofos, high-purity technology, applied in the field of profenofos preparation, can solve the problems such as the reduction of profenofos purity

Active Publication Date: 2012-08-01
山东科源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the existing profenofos production technology can only produce profenofos with a purity of about 90% by mass. The reason is that the raw material 2-chloro-4-bromophenol for producing profenofos contains 2-chloro-6-bromophenol Phenol and polybrominated by-products, by-products in these raw materials can reduce the purity of profenofos

Method used

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  • Preparation method of high-purity profenofos

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Embodiment 1

[0023] 1) O-chlorophenol and Br with a molar ratio of 1:1 2 reaction, the reaction temperature is 30°C, and the reaction time is 25 hours to obtain a brominated product, wherein the brominated product includes 94-95 mass % of 2-chloro-4-bromophenol and 3-4 mass % of by-product 2-chloro -6-bromophenol and 2-3% by mass of polybrominated by-products;

[0024] 2) Recrystallization: Slowly heat the brominated product obtained in step 1, so that the brominated product is heated up at a rate of 0.8°C / hour, stop heating when the brominated product temperature reaches 48°C, and then naturally cool down until the brominated product temperature reaches 42 ℃, the above-mentioned process of slowly heating up and then naturally cooling down is called the recrystallization process, and repeat the recrystallization process 2 times; repeated recrystallization 3 times can separate part of 2-chloro-6-bromophenol and polyphenol from the brominated product. Brominated by-products, the purity of 2...

Embodiment 2

[0030] 1) O-chlorophenol and Br with a molar ratio of 1:1 2 reaction, the reaction temperature is 50°C, and the reaction time is 20 hours to obtain brominated products, wherein the brominated products include 94-95% by mass of 2-chloro-4-bromophenol and 3-4% by-product 2-chloro -6-bromophenol and 2-3% by mass of polybrominated by-products;

[0031] 2) Recrystallization: Slowly heat the brominated product obtained in step 1) to raise the temperature of the brominated product at a rate of 1.0°C / hour, stop heating until the temperature of the brominated product reaches 50°C, and then cool down naturally until the temperature of the brominated product reaches 43 ℃, the above-mentioned process of slowly heating up and then naturally cooling down is called the recrystallization process, and repeat the recrystallization process 4 times; repeated recrystallization 5 times can separate part of 2-chloro-6-bromophenol and polyphenols from brominated products. Brominated by-products, the...

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Abstract

The invention relates to a preparation method of high-purity profenofos. The preparation method improves purity of 2-chloro-4-bromophenol by repeated recrystallization, and the purity of profenofos prepared by the method can reach 96 mass%. The preparation method comprises the following steps: (1) brominating; (2) recrystalizing for 3-5 times; (3) enabling O,O-diethyl sulfo phosphoryl chloride to react with a recrystalized bromination product to obtain O,O-diethyl-O-(2-chloro-4-bromophenyl)-phosphorothioate; (4) in the presence of trimethylamine, obtaining O-ethyl-O-(2-chloro-4-bromophenyl) thiophosphoric acid trimethylamine by backflow of O,O-diethyl-O-(2-chloro-4-bromophenyl)-phosphorothioate, and obtaining amine salt intermediates by dehydration and trimethylamine removal; (5) adding bromopropane and catalyst dimethyl formamide into the product obtained in the step (4) to react so that profenofos is formed; and (6) carrying out layering, washing and solvent removal to the product obtained in the step (5), and obtaining a profenofos product.

Description

technical field [0001] The invention relates to a preparation method of profenofos. Background technique [0002] Profenofos, or O-(4-bromo-2-chlorophenyl)-O-ethyl-S-n-propyl phosphorothioate, is a propylthio-containing phosphorothioate insecticide , has the characteristics of high efficiency and broad spectrum, has strong contact and stomach poisoning effects, and can kill insects and eggs. It has a good control effect on cotton bollworm, pink bollworm, cotton aphid, tobacco armyworm, spider mites, whitefly and other pests in cotton, fruit trees, rice, wheat, soybean, corn and other crops. Due to its unique mechanism of action, it shows high activity against resistant pests, especially the control effect of resistant cotton bollworm. Its structural formula is as follows: [0003] [0004] However, the existing profenofos production technology can only produce profenofos with a purity of about 90% by mass. The reason is that the raw material 2-chloro-4-bromophenol for ...

Claims

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Application Information

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IPC IPC(8): C07F9/18
Inventor 曲江升
Owner 山东科源化工有限公司
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