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In a 10L three-necked flask was charged water 1420g, sulfuric acid 2440g, glacial acetic acid 150mL slowly added 6- (trifluoromethyl) nicotinonitrile 870g (5mol).Reflux overnight reaction.Cool, add ice and cool with ice-brine to precipitate a white solid.The filtrate was extracted with ethyl acetate. The organic phases were combined, washed twice with water and the organic phase was dried to dryness and acid-washed to give 930 g of 6-(trifluoromethyl)-3-picolinic acid as a beige solid. The yield was 97.3%.
97.3%
With sulfuric acid; acetic acid; In water;Reflux;
In a 10 L three-necked flask, 1420 g of water, 2440 g of sulfuric acid and 150 mL of glacial acetic acid were added, and 870 g (5 mol) of 6- (trifluoromethyl) nicotinonitrile was added slowly.Reflux overnight reaction. Cooling, adding ice cubes, and cooling with ice brine, precipitating a white solid was filtered, the filtrate was extracted with ethyl acetate, the organic phases were combined, washed twice with water, the organic phase was dried and swirled,The residue was acid washed to give 930 g of 5- (trifluoromethyl) picolinic acid as an off-white solid in a yield of 97.3%.
97.3%
With sulfuric acid; acetic acid;Reflux;
Add 1420g of water to a 10L three-necked bottle,2440g sulfuric acid, 150mL glacial acetic acid,870 g (5 mol) of 6- (trifluoromethyl) nicotinonitrile was slowly added.The reaction was refluxed overnight.Cool down,Add ice cubes,And cooled with ice brine,A white solid precipitated.filter,The filtrate was extracted with ethyl acetate,Combined organic phases,Washed twice,The organic phase is dried and steamed,Acid-eluting color gives off-white solid930g of 5- (trifluoromethyl) picolinic acid,The yield was 97.3%
With hydrogenchloride; ammonium hydroxide; In water;
Reference Example 13 6-Trifluoromethylnicotinic acid A 2.9 g portion of <strong>[216431-85-5]5-cyano-2-trifluoromethylpyridine</strong> and 30 ml of concentrated hydrochloric acid were stirred at 90C for 13 hours. The reaction mixture was spontaneously cooled to room temperature, mixed with water and then adjusted to pH 2 to 3 with 28% aqueous ammonia. The thus precipitated crystals were collected by filtration and then washed with water to obtain 2.22 g of the title compound.
Reference Example 13 6-Trifluoromethylnicotinic acid A 2.9 g portion of <strong>[216431-85-5]5-cyano-2-trifluoromethylpyridine</strong> and 30 ml of concentrated hydrochloric acid were stirred at 90 C. for 13 hours.. The reaction mixture was spontaneously cooled to room temperature, mixed with water and then adjusted to PH 2 to 3 with 28% aqueous ammonia.. The thus precipitated crystals were collected by filtration and then washed with water to obtain 2.22 g of the title compound.
185 g
With formic acid; sulfuric acid; In water; at 0℃;Reflux;
2000 g of water was added to a three-necked flask, and 400 g of sulfuric acid and 80 g of formic acid were slowly added dropwise at 0 C. After stirring for 30 minutes, 200 g of <strong>[216431-85-5]6-(trifluoromethyl)nicotinonitrile</strong> was slowly added.After the addition is completed, the temperature is slowly raised and refluxed overnight.The TLC monitors the reaction of the starting material to a temperature of 0 C, and a white solid precipitates during the stirring. After filtration, the filtrate is extracted three times with 500 mL of ethyl acetate.Combine the organic phase,Wash 3000mL of water twice,Drying of the organic phase to give a white solid
In a 10 L three-necked flask, 1420 g of water, 2440 g of sulfuric acid, and 150 mL of glacial acetic acid were added, and 870 g (5 mol) of <strong>[216431-85-5]6-(trifluoromethyl)nicotinonitrile</strong> was slowly added thereto.The reaction was refluxed overnight.The temperature was lowered, ice was added, and cooled with iced brine to precipitate a white solid.After filtration, the filtrate was extracted with ethyl acetate. The organic phases were combined and washed twice with water. The organic phase was dried by rotary evaporation and the acid eluted to give 930 g of 6-(trifluoromethyl)picolinic acid as an off-white solid. The yield was 97.3%.
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