Preparation method of 2,3,5,6-tetraaminopyridine
A technology of tetraaminopyridine and dinitropyridine, which is applied in the field of polymer monomer 2, can solve problems such as unsafe conditions, and achieve the effects of mild conditions, high product purity, and safe and easy operation
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Embodiment 1
[0026] Add 39.8g (0.20mol) of 2,6-diamino-3,5-dinitropyridine, 50.5g (0.80mol) of anhydrous ammonium formate, and 200ml of anhydrous methanol in a reaction flask equipped with a stirrer and a thermometer, Add 2.0 g of 10% Pd / C, under normal pressure, stir at room temperature, control the reaction temperature at 20-45° C., and react for 40-50 minutes (track the reaction progress with thin-layer chromatography).
[0027] The reaction solution was filtered to remove the catalyst, the filter cake was washed with 30ml of anhydrous methanol, and the methanol was evaporated under reduced pressure (methanol was recovered and reused), washed with 120ml of water for 3 times, filtered, and dried to obtain 2, 3, 5, and 6 -Tetraaminopyridine crude product 27.1g, add 60ml of ethanol solvent, heat to dissolve, add 3g of activated carbon to decolorize, heat filter, pour the filtrate into 75ml of petroleum ether (60~90°C) to cool, filter out the precipitated crystals, dry to obtain 23.8 g of o...
Embodiment 2
[0029] Add 2,6-diamino-3,5-dinitropyridine 79.6g (0.40mol) in the reaction flask equipped with stirrer and thermometer, 201.8g (3.20mol) of anhydrous ammonium formate, 650ml absolute ethanol, Add 7.0g of 5% Pd / C, under normal pressure, stir at room temperature, control the reaction temperature at 20-45°C, and react for 45-60 minutes (track the reaction progress with thin-layer chromatography).
[0030] The reaction solution was filtered to remove the catalyst, the filter cake was washed with 50ml of absolute ethanol, and the ethanol was evaporated under reduced pressure (the ethanol was recovered and reused), washed with 300ml / time of water respectively for 3 times, filtered, and dried to obtain 2, 3, 5, 6 -Tetraaminopyridine crude product 55.1g, add 200ml isopropanol solvent, heat to dissolve, add activated carbon 6g to decolorize, hot filter, filtrate is poured in 200ml toluene, cool, filter out the crystal that separates out, dry, obtain off-white target product 52.6 g of 2...
Embodiment 3
[0032] Add 79.6g (0.40mol) of 2,6-diamino-3,5-dinitropyridine, 151.3g (2.40mol) of anhydrous ammonium formate, and 200ml of anhydrous methanol in a reaction flask equipped with a stirrer and a thermometer, Add 5.6g of 10% Pd / C to 300ml of isopropanol, under normal pressure, stir at room temperature, control the reaction temperature at 20-45°C, and react for 50-70 minutes (track the reaction process with thin-layer chromatography).
[0033] The reaction solution was filtered to remove the catalyst, the filter cake was washed with 50ml of anhydrous methanol, and the methanol was evaporated under reduced pressure (methanol was recovered and reused), washed with 300ml of water for 3 times, filtered, and dried to obtain 2, 3, 5, and 6 - Add 53.8g of tetraaminopyridine crude product into 200ml of isopropanol solvent, heat to dissolve, add 6g of activated carbon for decolorization, heat filter, pour the filtrate into 200ml of petroleum ether (60-90°C), cool, and filter out the precipi...
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