Pyridine-2,6-dicarboxylic acid synthesis
- Product Name:Pyridine-2,6-dicarboxylic acid
- CAS Number:499-83-2
- Molecular formula:C7H5NO4
- Molecular Weight:167.12
2402-78-0
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124-38-9
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499-83-2
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Yield:499-83-2 94.5%
Reaction Conditions:
Stage #1: 2,6-dichloropyridinewith magnesium;ethylene dibromide in tetrahydrofuran at 55; for 6 h;Inert atmosphere;
Stage #2: carbon dioxide in tetrahydrofuran at -15;Inert atmosphere;Acidic conditions;Temperature;Reagent/catalyst;Time;
Steps:
1 Example 1
148 g (1 mol) of 2,6-dichloropyridine was dissolved in a solution of 721 g (10 mol) of tetrahydrofuran. 60 g (2.5 mol) of magnesium powder was added. The nitrogen gas was vented. Stirring the case of heating solution to 55°C (ie, 2,6-dichloropyridine and active metal temperature 55°C). 0.55 g (0.005 mol) of the initiator, 1,2-dibromoethane. The reaction was carried out with stirring for 6 hours (i.e., the reaction time of 2,6-dichloropyridine and active metal was 6 hours). The reaction solution is transparent; Cooling to -15°C, the excessively dried carbon dioxide gas was slowly introduced. The reaction was judged on the basis of the flow rate of carbon dioxide when the incoming carbon dioxide and the same amount of exhaust gas to determine the end of the reaction. After the solution was acidified. Filter. Removal of tetrahydrofuran to give 2,6-pyridinedicarboxylic acid. The yield was 94.5%. After extraction, the purity was 97%.
References:
CN106187875,2016,A Location in patent:Paragraph 0020; 0021
108-48-5
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499-83-2
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