Method for synthesizing 2,6-dipicolinic acid
A technology of dipicolinic acid and dichloropyridine, which is applied in the development of pharmaceutical intermediates and pesticide fields, can solve the problems of high price and high cost, and achieve the effects of large cost advantage, low environmental pollution and environmental friendliness.
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Embodiment 1
[0021] 148g (1mol) 2,6-dichloropyridine was dissolved in 721g (10mol) tetrahydrofuran solution, 60g (2.5mol) magnesium powder was added, nitrogen was introduced to isolate the air, and the solution was heated while stirring to 55°C (ie 2, The reaction temperature of 6-dichloropyridine and active metal is 55℃), 0.55g (0.005mol) of initiator dibromoethane is added, and the reaction is carried out with stirring for 6 hours (that is, the reaction time of 2,6-dichloropyridine and active metal is 6 hours), the solution after the reaction is transparent; the temperature is lowered to -15°C, and excessive dry carbon dioxide gas is slowly introduced. The reaction is judged according to the carbon dioxide flow rate. When the amount of carbon dioxide and the exhaust gas are the same, the reaction is judged to be over, and the solution is acidified after the end , Filter and remove tetrahydrofuran to obtain 2,6-pyridinedicarboxylic acid with a yield of 94.5% and a purity of 97% after extrac...
Embodiment 2
[0023] Except that before adding the initiator, the solution was heated to 30°C (that is, the temperature of 2,6-dichloropyridine and the active metal is 30°C), and the rest of the reaction conditions are exactly the same as in Example 1. After the reaction, 2, The yield of 6-pyridinedicarboxylic acid was 92%, and the purity after extraction was 75.2%.
Embodiment 3
[0025] Except that before adding the initiator, the solution was heated to 60°C (that is, the temperature of 2,6-dichloropyridine and the active metal is 60°C), the rest of the reaction conditions are exactly the same as in Example 1. After the reaction, 2 ,6-pyridinedicarboxylic acid, the yield was 93.8%, and the purity after extraction was 94.3%.
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