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Method for converting cyanopyridine compounds into niacinamide compounds, its catalyst and the catalyst preparation
A catalyst, nicotinamide technology, applied in the preparation of nicotinamide compounds and isonicotinamide compounds, the preparation of anti-TB drugs - isoniazid, nicotinamide and isonicotinamide catalyst field, can solve the problem of high catalyst content , harm to the ecological environment, low yield of isonicotinamide, etc.
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Embodiment 1
[0033] Under constant stirring at 80°C, 125 ml of an aqueous solution containing 0.471 mol of manganese sulfate was added dropwise to 150 ml of an aqueous solution containing 0.395 mol of potassium permanganate within 1 hour, and allowed to stand for 15 hours. The resulting MnO 2 The precipitate was filtered and washed with distilled water until the filtrate was sulfate free. The precipitate was dried in an oven at 110° C. for 3 hours. The observed amount of manganese dioxide was 0.1497 moles.
[0034] Dissolve 0.096 mol of 3-cyanopyridine in 5.556 mol of water and add 0.0115 mol of MnO prepared by the above method 2 . The mixture was refluxed at 105°C for 8 hours. The reaction mixture was cooled and filtered. The filtrate was evaporated to dryness to obtain 0.095 mol of solid nicotinamide. The yield of isonicotinamide was 98.9 mol%.
Embodiment 2
[0036] Under vigorous stirring at 70°C, 115 ml of an aqueous solution containing 0.649 moles of potassium permanganate was added dropwise to 225 ml of an aqueous solution containing 0.5 moles of manganese chloride. The dropwise addition was continued for 1 hour and left to stand for 15 hours. The resulting manganese dioxide precipitate was filtered, and washed with distilled water until it contained no chloride ions. The precipitate was dried in an oven at 110° C. for 3 hours. The amount of manganese dioxide was 0.189 moles.
[0037] Dissolve 0.096 mol of 3-cyanopyridine in 4.55 mol of water and add 0.0115 mol of MnO prepared as above 2 . The mixture was refluxed at 100°C for 13.5 hours. The reaction mixture was cooled and filtered. The filtrate was evaporated to dryness to obtain 0.0879 moles of solid nicotinamide. The yield of nicotinamide was 91.56 mol%.
Embodiment 3
[0039] Under continuous stirring at 30°C, 225 ml of an aqueous solution containing 0.332 moles of potassium permanganate was added to 100 ml of an aqueous solution containing 1.125 moles of manganese chloride. The product, manganese dioxide, was filtered and washed with distilled water until it was free of chloride ions. The manganese dioxide precipitate was dried in an oven at 110° C. for 4 hours. The amount of manganese dioxide was 0.23 moles.
[0040] 0.096 mol of 3-cyanopyridine was dissolved in 5.556 mol of water, and 0.0115 mol of manganese dioxide prepared as described above was added to this solution. The mixture was stirred and refluxed at 100°C for 8 hours. The reaction mixture was cooled, filtered and washed thoroughly with distilled water. The filtrate was evaporated to dryness on a steam bath. The amount of nicotinamide after drying was 0.0957 mol, corresponding to a yield of 99.6 mol%.
[0041] Preparation of MnO using potassium permanganate and manganese sa...
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