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ChemicalBook CAS DataBase List Nicotinic acid
59-67-6

Nicotinic acid synthesis

14synthesis methods
Nicotinic acid, pyridine-3-carboxylic acid (20.2.9) is synthesized industrially by heating a paraldehyde trimer of acetaldehyde, under pressure with ammonia, which leads to the formation of 2-methyl-5-ethylpyridine, followed by oxidation with nitric acid which gives the desired product.

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Yield:59-67-6 99.58%

Reaction Conditions:

with oxygen;V2O5/Sb2O3-TiO2 in water at 260 - 280;Industry scale;Inert atmosphere;Gas phase;

Steps:

8

The catalyst was prepared by the method as described in Example 3 and process conditions were maintained as per Example 5 except that the process was carried out at large scale. The catalyst was packed as per Example 5 in a tubular reactor. Total volume of the reactor was 75 liters and equipped with heating and cooling arrangement. The catalyst bed was heated in the presence of air/nitrogen to 250° C. β-picoline, water and air were fed separately through a vaporizer from top of the reactor. The molar feed ratio of oxygen:water:β-picoline was 20:40:1 and WHSV was 0.05 hr-1. The nicotinic acid was isolated by the method as described in Example 4. The vent gases and scrubbed liquid obtained from secondary absorber and mother liquor of first absorber was recycled back in the process with optimum purge. The nicotinic acid obtained was white colored. Selectivity: 90.8%; β-picoline conversion of 94.6%. Assay: 99.58%.

References:

US2012/65405,2012,A1 Location in patent:Page/Page column 5

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