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Preparation method of boscalid

A technology of boscalid and formamide, which is applied in the field of fungicide preparation, can solve the problems of low yield, high cost, and harsh reaction conditions, and achieve the effects of high yield, low cost, and reduced production cost

Active Publication Date: 2015-11-25
利民化学有限责任公司
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Problems solved by technology

[0004] In order to solve the shortcomings of the prior art such as low yield, high cost, and harsh reaction conditions, the present invention provides a preparation method for boscalid, which uses Ni / C as a catalyst to carry out Suzuki coupling reaction greatly reduces the production cost, and the production raw materials are easy to obtain, the yield is high, and it is suitable for large-scale industrial production

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  • Preparation method of boscalid
  • Preparation method of boscalid
  • Preparation method of boscalid

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Embodiment

[0019] 1. Preparation of Ni / C catalyst

[0020] (1) After vacuuming 900g of activated carbon (20-40 mesh) for half an hour, immediately put it into Ni(NO) with a concentration of 0.8mol / L 3 ) 2 ·6H 2 O methanol immersion solution 1L, let stand for 24h at room temperature, and then load Ni(NO 3 ) 2 The activated carbon was dried at 120°C for 8 hours and then placed in a desiccator for later use.

[0021] (2) Load Ni(NO 3 ) 2 Activated carbon in N 2 In an atmosphere, it was heated to 500°C at a heating rate of 10°C / min, and calcined at a constant temperature of 500°C for 3 hours, and then slowly cooled to room temperature, to obtain 945 g of Ni / C catalyst. (The content of Ni is about 5%)

[0022] 2. Preparation of boscalid

[0023] Add 2-chloronicotinic acid chloride (77.44g, 440mmol), o-iodoaniline (88.5g, 400mmol), triethylamine (3ml) and dichloroethane (450mL) into a 2L three-necked flask, stir at 0℃ for 6h, and react After the completion, first wash with water (30mL), then with hyd...

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Abstract

A preparation method of boscalid comprises following steps: o-iodoaniline and 2-chloronicotinyl chloride have a condensation reaction to produce an intermediate product 2-chloro-N-(2-iodophenyl)pyridine-3-formamide;2-chloro-N-(2-iodophenyl)pyridine-3-formamide which is not purified has a Suzuki coupling reaction with 4-chlorophenylboronic acid directly, and boscalid is produced. A Ni / C preparation method is provided, and Ni / C is taken as a catalyst for the Suzuki coupling reaction, so that the production cost is greatly reduced; further, production raw materials are available, the yield is high, and the preparation method of boscalid is applicable to large-scale industrial production.

Description

Technical field [0001] The invention relates to a preparation method of a bactericide, in particular to a preparation method of boscalid. Background technique [0002] The full name of boscalid is N-(4'-chloro-2-biphenyl)-2-chloro-3-pyridinecarboxamide, which is a highly effective bactericide. The first is the new varieties of fungicides registered by BASF of Germany and AG of Japan in more than 50 countries including Europe and the United States. It is mainly used to prevent gray mold and sclerotinia disease of vegetables and beans. The mechanism of action is that the medicinal solution is absorbed by the plant and penetrates through the leaf surface, and then is transferred in the plant, which can inhibit the activity of mitochondrial succinate dehydrogenase, thereby hindering the tricarboxylic acid cycle, causing the lack of amino acids, sugar, energy, and interference with cells It has bactericidal activity by dividing and growing. The boscalid synthesis method reported in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/82A01N43/40A01P3/00
CPCA01N43/40C07D213/82
Inventor 孙敬权冯小冬陈浩孙丽梅
Owner 利民化学有限责任公司
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