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The 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: 2018-09-25
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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  • The preparation method of boscalid
  • The preparation method of boscalid
  • The preparation method of boscalid

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Experimental program
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Embodiment

[0019] 1. Preparation of Ni / C catalyst

[0020] (1) After evacuating 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 impregnation solution 1L, at room temperature for 24h, and then loaded with Ni(NO 3 ) 2 The activated carbon was dried at 120°C for 8 h and placed in a desiccator for later use.

[0021] (2) Load Ni(NO 3 ) 2 activated carbon, in N 2 Under the 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 945g of Ni / C catalyst. (Ni content is about 5%)

[0022] 2. Preparation of boscalid

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

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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 fungicide, 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 fungicide. The first is a new type of fungicide 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 control gray mold and sclerotinia of vegetables and beans. Its mechanism of action is that the medicinal liquid is absorbed by the plant and permeated through the leaves, and then transferred in the plant, which can inhibit the activity of mitochondrial succinate dehydrogenase, thereby hindering the tricarboxylic acid cycle, causing amino acid and sugar deficiency, reducing energy, and interfering with cells. The division and growth have fungicidal activity. The boscalid synthesis method reported in the literature is di...

Claims

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Application Information

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Patent Type & Authority Patents(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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