A synthetic method of N-cyanomethyl-4-(trifluoromethyl)nicotinamide
The technology of a trifluoromethyl group and a synthetic method, applied in the field of pesticides, can solve the problems of high production safety risks and the like, and achieve the effects of convenient operation, simple process and good yield
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Embodiment 1
[0027] After adding 19g (0.1mol) of 4-(trifluoromethyl)nicotinamide, 12.72g (0.12mol) of sodium carbonate and 80g of dimethylformamide in a 250mL reactor with a reflux condenser, at 15± 8.25 g (0.11 mol) of chloroacetonitrile was added dropwise with stirring at 5°C, and then the reaction temperature was raised to 80°C for 8 hours.
[0028] After the reaction, the liquid layer was analyzed by liquid chromatography, and the result was that the yield (selectivity) of N-cyanomethyl-4-(trifluoromethyl)nicotinamide was 96.8%, and 4-(trifluoromethyl) ) The conversion rate of nicotinamide is 98.9%, and the yield is selectivity, which is the converted yield without separation and purification.
Embodiment 2
[0030] After adding 19g (0.1mol) of 4-(trifluoromethyl)nicotinamide, 15.9g (0.15mol) of sodium carbonate and 100g of dimethylformamide in a 250mL reactor with a reflux condenser, at 15± 8.25 g (0.11 mol) of chloroacetonitrile was added dropwise with stirring at 5°C, and then the reaction temperature was raised to 80°C for 8 hours.
[0031] After the reaction, the liquid layer was analyzed by liquid chromatography, and the result was that the yield (selectivity) of N-cyanomethyl-4-(trifluoromethyl)nicotinamide was 96.5%, and 4-(trifluoromethyl) ) The conversion rate of nicotinamide is 98.6%, and the yield is selectivity, which is the converted yield without separation and purification.
Embodiment 3
[0033] After adding 19g (0.1mol) of 4-(trifluoromethyl)nicotinamide, 15.9g (0.15mol) of sodium carbonate and 100g of dimethylformamide in a 250mL reactor with a reflux condenser, at 15± 11.25 g (0.15 mol) of chloroacetonitrile was added dropwise with stirring at 5°C, and then the reaction temperature was raised to 80°C for 8 hours.
[0034] After the reaction, the liquid layer was analyzed by liquid chromatography, and the result was that the yield (selectivity) of N-cyanomethyl-4-(trifluoromethyl)nicotinamide was 96.2%, and 4-(trifluoromethyl) ) The conversion rate of nicotinamide is 98.1%, and the yield is selectivity, which is the converted yield without separation and purification.
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