2-ACETONICOTINIC ACID synthesis
- Product Name:2-ACETONICOTINIC ACID
- CAS Number:89942-59-6
- Molecular formula:C8H7NO3
- Molecular Weight:165.15
611-32-5
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Yield: 70%
Reaction Conditions:
Stage #1:8-methylquinoline with sulfuric acid;oxygen;ozone in water at 1;
Stage #2: with air in water at 60; for 2 h;
Stage #3: with sodium hydroxide in water
Steps:
3 EXAMPLE 3
250 kg of 8-methylquinoline (1.75 kmol) were dissolved in 3200 liters of water and 180 kg of 96% strength sulfuric acid (1.75 kmol).. The solution was cooled to a temperature of 1° C., and then a stream of oxygen which contained 50 to 60 g/M3 of ozone was introduced.. This was continued until the residual content of 8-methylquinoline was about 1 gram/liter (determination by means of GC).. After the ozonolysis, the reaction mixture was let down into a reactor which contained 2000 liters of water at a temperature of 60° C. 2 m3 of air per hour were continuously introduced into the aqueous solution during the peroxide decomposition.. The peroxide decomposition was carried out for 2 hours at a temperature of 60° C. until the peroxide residue content was 3 to 5 mmol/liter (titration).. 50% strength sodium hydroxide solution was used to establish a PH of from 1.5 to 2, and the solution was extracted countercurrently with methyl tert-butyl ether in the methyl tert-butyl ether/aqueous solution phase ratio=1.5/1 using a sieve-plate extractor.. The extract was concentrated to a concentration of about 10% by weight by distilling off methyl tert-butyl ether.. The solution was cooled to -10° C., and the product was filtered over a pressure filter, washed with prechilled methyl tert-butyl ether and dried on the filter in vacuo. This gave 202 kg (70% of theory) of 2-acetyl-nicotinic acid.. According to HPLC, the purity was 98.5%; no 2-acetyl-4-methylnicotinic acid was detectable as byproduct.
References:
DSM Fine Chemicals Austria Nfg GmbH & CoKG US6346623, 2002, B1 Location in patent:Page column 4-5
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