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N-cyanomethyl-4-(trifluoromethyl) nicotinamide preparation method

A technology of trifluoromethyl and cyanomethyl, applied in the field of preparation of N-cyanomethyl-4-(trifluoromethyl)nicotinamide, can solve the problems of high production cost, difficult industrialization, low yield and the like, Achieve the effect of low production cost, easy operation and high yield

Active Publication Date: 2018-11-27
山东沾化永浩医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The object of the present invention is to provide a kind of N-cyanomethyl-4-(trifluoromethyl)nicotinamide to overcome the problems of low yield, difficult purification, high production cost and difficulty in industrialization in the preparation of existing N-cyanomethyl-4-(trifluoromethyl)nicotinamide. The preparation method of methyl-4-(trifluoromethyl)nicotinamide

Method used

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Examples

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Effect test

Embodiment 1

[0024] Put 30.0 g (0.157 mol) of 4-(trifluoromethyl) nicotinic acid and 100 ml of benzene into a 250 ml four-neck flask equipped with a reflux condenser, a thermometer, and a dropping funnel, heat up to 50-60 ° C, drop Add 28.0 g (0.235 mol) of thionyl chloride for about 1 hour. After the dropwise addition, the temperature is raised to 80° C. and kept for 2 hours. After the reaction is completed, 4-(trifluoromethyl)nicotinoyl chloride benzene solution is obtained for later use.

[0025] In another 1000 ml four-necked flask with a thermometer and a dropping funnel, 33.3 grams (0.314 mol) of sodium carbonate and 133.2 grams of tap water were put in, and after stirring for 10 minutes, 120 ml of benzene and 21.79 grams of aminoacetonitrile hydrochloride (0.235 mol), then the temperature was lowered to 10°C under stirring, and the 4-(trifluoromethyl)nicotinoyl chloride benzene solution was added dropwise, and the addition was completed in about 3 hours, and the temperature was kept ...

Embodiment 2

[0027] Put 30.0 g (0.157 mol) of 4-(trifluoromethyl) nicotinic acid and 100 ml of toluene into a 250 ml four-necked flask equipped with a reflux condenser, a thermometer, and a dropping funnel, heat up to 50-60 ° C, drop Add 28.0 g (0.235 mol) of thionyl chloride for about 1 hour. After the dropwise addition, the temperature is raised to 80° C. and kept for 2 hours. After the reaction is completed, 4-(trifluoromethyl)nicotinoyl chloride benzene solution is obtained for later use.

[0028] In another 1000 ml four-necked flask with a thermometer and a dropping funnel, 33.3 grams (0.314 mol) of sodium carbonate and 133.2 grams of tap water were put in, and after stirring for 10 minutes, 120 milliliters of toluene and 21.79 grams of aminoacetonitrile hydrochloride (0.235 mol), then the temperature was lowered to 10°C under stirring, and the 4-(trifluoromethyl)nicotinoyl chloride benzene solution was added dropwise, and the addition was completed in about 3 hours, and the temperatur...

Embodiment 3

[0030] 30.0 g (0.157 mol) of 4-(trifluoromethyl) nicotinic acid and 100 ml of dichloroethane were put into a 250 ml four-neck flask with a reflux condenser, a thermometer, and a dropping funnel, and the temperature was raised to 50-60 ℃, add 28.0 g (0.235 mol) of thionyl chloride dropwise, and finish adding in about 1 hour. After the dropwise addition is completed, raise the temperature to 80°C and keep it for 2 hours. After the reaction is completed, 4-(trifluoromethyl)nicotinoyl chloride benzene solution is obtained .

[0031] In another 1000 ml four-necked flask with a thermometer and a dropping funnel, put 33.3 grams (0.314 mol) of sodium carbonate and 133.2 grams of tap water into it. After stirring for 10 minutes, put 120 milliliters of dichloroethane and 21.79 grams of aminoacetonitrile hydrochloride. gram (0.235mol), then lower the temperature to 10°C while stirring, and start to drop the 4-(trifluoromethyl)nicotinoyl chloride benzene solution for use in the previous s...

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Abstract

The invention belongs to the technical field of pesticide synthesis, in particular to an N-cyanomethyl-4-(trifluoromethyl) nicotinamide preparation method. The method includes the following steps: reacting, by 4-(trifluoromethyl) niacinamide, with thionyl chloride to obtain acyl chloride; and then reacting with aminoacetonitrile hydrochloride to synthesize the N--cyanomethyl-4-(trifluoromethyl) nicotinamide under an inorganic weak alkaline aqueous solution environment. According to the invention, the preparation method is simple in process, simple in operation, high in yield coefficient (be equal or greater than 92% of mole yield coefficient in terms of trifluoromethylnicotinamide), few in impurities, the purity can reach be equal or greater than 99. 5%, low in production costs, convenientfor solvent recovery, recyclable, less in pollution, high in safety, and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pesticide synthesis, and specifically relates to a preparation method of N-cyanomethyl-4-(trifluoromethyl)nicotinamide. Background technique [0002] N-cyanomethyl-4-(trifluoromethyl)nicotinamide is a new type of low-toxicity pyridine amide insect growth regulator insecticide. In 2007, it obtained the temporary registration certificate of pesticide products in my country. The preparation is 10% water dispersion granules. In addition to its contact and stomach poisoning effects, it also has a good nerve agent and rapid antifeedant effect. Aphids and other piercing-sucking mouthparts will be quickly prevented from sucking the juice after inhaling the plant juice with flonicamid. There will be no excrement at all within 1 hour, and eventually they will die of starvation. [0003] Its general chemistry test is as follows: [0004] [0005] The synthesis methods reported in literature at home and abroad m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 倪政
Owner 山东沾化永浩医药科技有限公司
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