ChemicalBook CAS DataBase List 4-(Trifluoromethyl)nicotinic acid

4-(Trifluoromethyl)nicotinic acid synthesis

12synthesis methods

Product Name:4-(Trifluoromethyl)nicotinic acid
CAS Number:158063-66-2
Molecular formula:C7H4F3NO2
Molecular Weight:191.11

synthesis of 4-(Trifluoromethyl)nicotinic acid: add 5g (0.0192mol) Methyl 2,6-dichloro-4-(trifluoromethyl)nicotinate in turn to a 100mL three-necked flask, 0.3g of 10% Pd/C (water content 63.45%) ), 5.25g (0.0389mol) CH3COONa 3H2O and 20mL ethanol, after stirring and dissolving, nitrogen was replaced 3 times to discharge air, after hydrogen replacement 2 times, the reaction was stirred at room temperature for 8h under a hydrogen atmosphere until no hydrogen was absorbed to complete the reaction, and suction filtration was recovered. Palladium carbon, washed the filter cake 3 times with ethanol, the filtrate was rotary evaporated to remove the solvent, added 20 mL of water to the obtained solid, fully shaken to dissolve it, added hydrochloric acid to adjust pH=2～3, extracted 3 times with ethyl acetate, The organic phases were combined and washed three times with saturated brine, dried over anhydrous sodium sulfate, and rotary-evaporated to obtain 3.3 g of a pale yellow solid with a yield of 90.4%.

13600-43-6 Synthesis

13600-43-6
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$32.00/1g

158063-66-2
377 suppliers
$5.00/250mg

Yield:158063-66-2 98.3%

Reaction Conditions:

with water;sodium hydroxide at 100;Temperature;

Steps:

9 Example 9: Preparation of 4-trifluoromethylnicotinic acid.
In a 1000 mL sealed four-neck reaction flask, add 150 g of sodium hydroxide and 500 mL of water, stir well,Further, 172.1 g of 4-trifluoromethyl cigarette obtained in the above Example 4 was added, and the mixture was stirred and controlled at a temperature of 100 ° C, and the solid was dissolved and turned into a pale yellow clear solution, then the stirring was stopped, the pH was adjusted with hydrochloric acid, and the mixture was cooled and filtered.The white solid was 187.9 g of 4-trifluoromethylnicotinic acid in a yield of 98.3%.

References:

Zhejiang University Of Technology Shangyu Institute Co., Ltd.;Fang Biao;Ke Junliang;Xu Meng CN109467532, 2019, A Location in patent:Paragraph 0034-0039

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158062-71-6 Synthesis