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Synthesis process of boscalid intermediate 2-(4-chlorphenyl)phenylamine

A technology for the synthesis of boscalid and boscalid, which is applied in the field of synthesis of boscalid intermediate 2-aniline, which can solve the problems of insufficient synthesis, low work efficiency, and low product yield, and achieve excellent workmanship and high work efficiency. High, guaranteed high yield effect

Inactive Publication Date: 2017-05-31
ZHEJIANG RONGKAI TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis process of boscalid preparations in China is not sophisticated enough, the output of the product is not high, and the work efficiency is low

Method used

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  • Synthesis process of boscalid intermediate 2-(4-chlorphenyl)phenylamine
  • Synthesis process of boscalid intermediate 2-(4-chlorphenyl)phenylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Under the protection of stirring and inert gas, put tert-butanol, water and potassium tert-butoxide into a stirred reaction vessel and stir fully to form a mixed solvent to be reacted, take out 100ml mixed solvent and add 30g o-chloronitrobenzene and 33g p-chloro Phenylboronic acid, stir well until the particles are all dissolved, continue to add a total of 1.5mg of Pd(OAc) to the mixed solvent 2 , 0.3mg of KI-based catalyst, fully stirred the temperature to 60°C and reacted for 4h, then cooled to 35°C, filtered to obtain the filtrate, and added 0.75mg of Pt-based catalyst to the filtrate, adjusted the temperature to 60°C and continued Hydrogen gas was introduced, and the finally obtained reaction solution was concentrated to 80° C. and cooled to obtain 35 g of finished product 2-(4-chlorophenyl)aniline, the content of which was 93.4% after detection.

Embodiment 2

[0031] Under the protection of stirring and inert gas, put tert-butanol, water and potassium tert-butoxide into a stirred reaction vessel and stir fully to form a mixed solvent to be reacted, take out 120ml mixed solvent and add 30g o-chloronitrobenzene and 35g p-chloro Phenylboronic acid, stir well until the particles are all dissolved, and continue to add a total of 3.5 mg of Pd(OAc) to the mixed solvent 2 , 0.6mg of KI-based catalyst, fully stirred the temperature to 80°C and reacted for 6h, then cooled to 40°C, filtered to obtain the filtrate, and added 1.75mg of Pt-based catalyst to the filtrate, adjusted the temperature to 80°C and continued Hydrogen gas was introduced, and the finally obtained reaction solution was concentrated to 70° C. and lowered in temperature to obtain 36 g of finished 2-(4-chlorophenyl)aniline, the content of which was 93.9% after detection.

Embodiment 3

[0033] Under the protection of stirring and inert gas, put tert-butanol, water and potassium tert-butoxide into a stirring reaction vessel and stir fully to form a mixed solvent to be reacted, take out 150ml mixed solvent and add 30g o-chloronitrobenzene and 40g p-chloro Phenylboronic acid, stir well until the particles are all dissolved, and continue to add a total of 3.5 mg of Pd(OAc) to the mixed solvent 2 , 0.3mg of KI-based catalyst, fully stirred the temperature to 90°C and reacted for 8h, then cooled to 45°C, filtered to obtain the filtrate, and added 1.75mg of Pt-based catalyst to the filtrate, adjusted the temperature to 90°C and continued Hydrogen gas was introduced, and the finally obtained reaction solution was concentrated to 90° C. and cooled to obtain 40 g of finished product 2-(4-chlorophenyl)aniline, the content of which was 94.5% after detection.

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Abstract

The invention discloses a synthesis process of boscalid intermediate 2-(4-chlorphenyl)phenylamine. Chlorophenylboronic acid and o-chloronitrobenzene are taken as starting raw materials, and a main reaction consisting of the two steps of Suziki and hydrogenation reduction is carried out to prepare the 2-(4-chlorphenyl)phenylamine. 1, optimal reaction steps determined through continuous testing are adopted, a proper solvent is selected preferably, and the 2-(4-chlorphenyl)phenylamine is prepared at a proper temperature and under a proper pressure, so that a superior process, high yield and high working efficiency are realized, no noble metal coupling agent is needed, the environmental pollution is lowered, raw materials are readily available, and the production cost is lowered; 2, a target product is obtained by obtaining a solid through concentration and cooling, so that a posttreatment method is simplified effectively, and meanwhile the content and high yield of the product are ensured effectively; 3, the Suzuki reaction steps are simple, filtrate left after the reaction can be directly applied to a next-step hydrogenation reduction reaction, operation is easy, no pollutant waste is produced in the hydrogenation reduction reaction, and the environment and the health of operating personnel are protected.

Description

technical field [0001] The invention relates to the technical field of medicines for treating blood fever in human body, in particular to a synthesis process of boscalid intermediate 2-(4-chlorophenyl)aniline. Background technique [0002] Boscalid (common name: Boscalid) is a new type of pyridine nicotinamide systemic fungicide developed by BASF in Germany. It is an inhibitor of succinate coenzyme Q reductase in the mitochondrial respiratory chain and has a strong inhibitory effect on the germination of spores. ability. The medicinal solution penetrates through the leaves and is absorbed by the plants, and then transferred in the plants, which can inhibit the activity of mitochondrial succinate dehydrogenase, thereby hindering the tricarboxylic acid cycle, causing the lack of amino acids and sugars, reducing energy, and interfering with cell division and growth And have bactericidal activity. Its unique mechanism of action, no cross-resistance with other drugs, and ecolog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/56
CPCC07C209/365C07C201/12C07F3/02C07F5/025
Inventor 张云文孙鑫李周方
Owner ZHEJIANG RONGKAI TECH DEV
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