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A kind of synthesis technique of boscalid

A synthesis process and boscalid technology are applied in the field of synthesis technology of broad-spectrum fungicide boscalid and related intermediates, and can solve problems such as high price, difficulty in increasing mass production, and increasing production cost, etc. Achieve the effect of low production cost, short synthesis route and simple post-processing

Active Publication Date: 2020-08-28
ANHUI THERAPY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] In summary, most of the reported synthetic processes of boscalid use expensive catalysts, which greatly increases the production cost and increases the difficulty of mass production

Method used

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  • A kind of synthesis technique of boscalid
  • A kind of synthesis technique of boscalid
  • A kind of synthesis technique of boscalid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 27.5g of o-chlorobenzonitrile and 156g of benzene were mixed into the reaction flask, and 74g of potassium tert-butoxide was added, and then 1.38g of activated carbon-supported Rh 2 Cl 2 (cod) 2 added to the reaction system. The system was stirred at 70 °C for 24 h. After the reaction, the catalyst was filtered out for reuse. The reaction solution was washed once with 200 mL of water, and the organic phase was distilled directly to recover the excess benzo and obtain 26.7 g of the product 2-cyanobiphenyl as an off-white solid with a melting point of 34-37 degrees. 1H NMR (400MHz, CDCl3) δ7.71-7.76 (m, 1H), 7.62 (d, J=1.2Hz, 1H), 7.58-7.56 (m, 2H), 7.50-7.42 (m, 5H).

Embodiment 2

[0058] 27.5g of o-chlorobenzonitrile and 15.6g of benzene were dissolved in 170ml of tetrahydrofuran, and 74g of potassium tert-butoxide was added, and then 1.38g of activated carbon-supported PdCl was added under nitrogen protection. 2 (cod) 2 added to the reaction system. The system was stirred at 70 °C for 24 h. After the reaction, the catalyst was filtered out for reuse. The reaction solution was washed once with 200 mL of water, and the organic phase was directly distilled to recover excess benzene and obtain 2.1 g of off-white solid 2-cyanobiphenyl.

Embodiment 3

[0060] 27.5g of o-chlorobenzonitrile and 156g of benzene were mixed into the reaction flask, and 41g of sodium ethoxide was added, and then 1.38g of activated carbon-supported Rh 2 Cl 2 (cod) 2 added to the reaction system. The system was stirred at 70 °C for 24 h. After the reaction, the catalyst was filtered out for reuse. The reaction solution was washed once with 200 mL of water, and the organic phase was distilled directly to recover excess benzene and obtain 13.2 g of off-white solid product 2-cyanobiphenyl.

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Abstract

The invention discloses a process for synthesizing boscalid. The process comprises the following steps: (1) coupling o-chlorobenzonitrile with benzene to obtain 2-cyanobiphenyl, then carrying out chlorination, reduction and salt formation purification to obtain 4'-chloro-2-aminobiphenyl hydrochloride; (2) carrying out condensation reaction on the prepared 4'-chloro-2-aminobiphenyl hydrochloride and 2-chloronicotinoyl chloride to obtain the boscalid. The process for synthesizing the boscalid has the advantages of simple synthesis process, no need of complex aftertreatment, cheap and easily available basic chemical raw materials, and suitability for industrial production.

Description

Technical field: [0001] The invention relates to the field of pesticide fungicides, in particular to a synthesis process of the broad-spectrum fungicide boscalid and related intermediates. Background technique: [0002] Boscalid is a nicotinamide fungicide, which was first successfully developed by BASF in Germany. It has a wide bactericidal spectrum and has a preventive effect. It is active against almost all types of fungal diseases. It is effective in preventing and controlling powdery mildew, gray mold, Root rot, sclerotinia, and various rot diseases are very effective, and it is not easy to produce cross-resistance. It is also effective for resistant bacteria to other chemicals. It is mainly used for the prevention and control of diseases including rapeseed, grapes, fruit trees, vegetables, and field crops. . The test results show that boscalid has obvious control effect on Sclerotinia sclerotiorum, and the control effect of diseased plant rate and disease index contro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 孙玉行彭兵兵任磊张红夺何斌马恩源
Owner ANHUI THERAPY PHARMA CO LTD