Synthetic process of 5-bromo-3-methyl-1h-pyrazolo[3,4-b]pyridine
A synthesis process, pyrazolo technology, applied in the field of synthesis process of pyrazolo pyridine derivatives, can solve the problems of unfavorable large-scale production and application, low yield, etc., and achieve the effect of low cost and simple operation steps
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Embodiment 1
[0014] This example relates to a synthesis process of 5-bromo-3-methyl-1H-pyrazolo[3,4-B]pyridine, which consists of the following steps: 0.1mol 5-bromo-3-ethynyl-2 -Chloro-pyridine was put into a 500mL reaction bottle, added to 100mL DMF, and then sequentially added 0.1mol hydrazine, 0.05mol calcium carbonate and 0.008mol aluminum silicate, mixed evenly, then reacted at 4°C for 30 hours, filtered to remove insoluble matter, and Evaporate the solvent under pressure, recrystallize once with 50mL ethanol, and dry overnight at 35°C to obtain 18.2g of white 5-bromo-3-methyl-1H-pyrazolo[3,4-B]pyridine with a yield of 85.3% , purity 99.6%, MS: m / z=212 (M + ); 1 H-NMR (300 MHz, DMSO) δ: 8.16 (s, 1H), 7.58 (s, 1H), 1.05 (s, 3H).
Embodiment 2
[0016] This example relates to a synthesis process of 5-bromo-3-methyl-1H-pyrazolo[3,4-B]pyridine, which consists of the following steps: 0.1mol 5-bromo-3-ethynyl-2 -Chloro-pyridine was put into a 500mL reaction flask, added to 100mL DMF, then added 0.1mol hydrazine, 0.05mol calcium carbonate and 0.02mol aluminum silicate in sequence, mixed well, then reacted at 6°C for 24 hours, filtered to remove insoluble matter, and reduced Evaporate the solvent under pressure, recrystallize once with 50mL ethanol, and dry overnight at 35°C to obtain 17.6g of white 5-bromo-3-methyl-1H-pyrazolo[3,4-B]pyridine with a yield of 82.7% , purity 99.5%, MS: m / z=212 (M + ); 1 H-NMR (300 MHz, DMSO) δ: 8.16 (s, 1H), 7.57 (s, 1H), 1.04 (s, 3H).
Embodiment 3
[0018] This example relates to a synthesis process of 5-bromo-3-methyl-1H-pyrazolo[3,4-B]pyridine, which consists of the following steps: 0.1mol 5-bromo-3-ethynyl-2 -Chloro-pyridine was put into a 500mL reaction flask, added to 100mL DMF, and then sequentially added 0.1mol hydrazine, 0.05mol calcium carbonate and 0.003mol aluminum silicate, mixed well, then reacted at 2°C for 27 hours, filtered to remove insoluble matter, and Evaporate the solvent under pressure, recrystallize once with 50mL of ethanol, and dry overnight at 35°C to obtain 17.9g of white 5-bromo-3-methyl-1H-pyrazolo[3,4-B]pyridine with a yield of 84.1% , purity 99.6%, MS: m / z=212 (M + ); 1 H-NMR (300 MHz, DMSO) δ: 8.15 (s, 1H), 7.59 (s, 1H), 1.05 (s, 3H).
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