4-NITROPICOLINIC ACID synthesis
- Product Name:4-NITROPICOLINIC ACID
- CAS Number:13509-19-8
- Molecular formula:C6H4N2O4
- Molecular Weight:168.11
19235-88-2
13509-19-8
Synthesis of III-2-2:4-nitropyridine carboxylic acid 5.00 g (34 mmol) of 2-cyano-4-nitropyridine was dissolved in 50 g of 90% sulfuric acid and the reaction was stirred at 120°C for 2 hours. Subsequently, a solution of 5.60 g of sodium sulfite dissolved in 10 ml of water was slowly added dropwise at 20 °C to 25 °C, and the stirring was continued at the same temperature for 1 h. After that, the reaction was warmed up to 80 °C for 1 h. The reaction was completed by cooling to room temperature. Upon completion of the reaction, it was cooled to room temperature, diluted by adding 100 g of ice water, and the pH of the mixture was adjusted with sodium carbonate to about 2. The mixture was allowed to stand in a refrigerator to induce precipitation of solids. The precipitate was collected by filtration and recrystallized using a water-acetone solvent mixture to give 3.50 g of light yellow crystalline product in 62.1% yield. The melting point of the product was 157°-158°C (accompanied by decomposition).The IR (KBr) spectrum showed characteristic absorption peaks located at 1710, 1600, 1585, 1535 cm-1 .
1124-33-0
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13509-19-8
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Yield:-
Steps:
Multi-step reaction with 3 steps
1: 2 h / 65 - 70 °C
2: 73 percent / H2O / -8 - -7 °C
3: 1.) 90percent H2SO4, 2.) NaNO2 / 1.) 120 deg C, 2 h, 2.) water, 20-25 deg C, 1 h, then 80 deg C, 1 h
References:
Desjardins, Sylvie Y.;Cavell, Kingsley J.;Hoare, Jason L.;Skelton, Brian W.;Sobolev, Alexander N.;White, Allan H.;Keim, Wilhelm [Journal of Organometallic Chemistry,1997,vol. 544,# 2,p. 163 - 174]
19235-88-2
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13509-19-8
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13508-96-8
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13509-19-8
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18437-58-6
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13509-19-8
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694-59-7
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13509-19-8
156 suppliers
$30.00/250mg