Preparation method of sorafenib
A substance-to-quantity ratio technology, applied in organic chemistry and other directions, can solve the problems of unsuitable industrial production, expensive catalysts, difficult operation, etc., and achieve the effects of high conversion rate, saving solvent consumption cost, and high reaction yield.
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Embodiment 1-1
[0034] The synthesis of embodiment 1-1 intermediate I
[0035] In a 100mL three-neck flask equipped with a magnetic stirring device, a thermometer and a reflux condenser, add 105mmol of p-aminophenol, heat and melt, add 100mmol of KOH, react for 10min under stirring, and then add 90mmol of 4-chloro- N-methylpyridine-2-carboxamide, temperature-controlled reaction; the end point was detected by TLC, and the reaction ended in 1.5h; hot 5% NaOH solution was added to the reaction system, kept at 80°C to 85°C and washed 3 times, and then After washing with water at low temperature for 3 times, the reaction mixture was poured into cold water while it was hot, cooled, filtered, and dried to obtain 21.30 g of Intermediate I with a yield of 97.3% and a purity of 99.91%.
Embodiment 1-2
[0036] The synthesis of embodiment 1-2 intermediate I
[0037] In a 100mL three-neck flask equipped with a magnetic stirring device, a thermometer and a reflux condenser, add 90mmol of p-aminophenol, heat and melt, add 100mmol of KOH, react for 10min under stirring, and then add 100mmol of 4-chloro- N-methylpyridine-2-carboxamide, temperature-controlled reaction; the end point was detected by TLC, and the reaction ended in 1.5h; hot 5% NaOH solution was added to the reaction system, kept at 80°C to 85°C and washed 3 times, and then After washing with water at low temperature for 3 times, the reaction mixture was poured into cold water while it was hot, cooled, filtered, and dried to obtain 20.11 g of Intermediate I with a yield of 91.7% and a purity of 99.75%.
Embodiment 1-3
[0038] Synthesis of Example 1-3 Intermediate I
[0039] In a 100mL three-neck flask equipped with a magnetic stirring device, a thermometer and a reflux condenser, add 120mmol of p-aminophenol, heat and melt, add 100mmol of KOH, react for 10min under stirring, and then add 80mmol of 4-chloro- N-methylpyridine-2-carboxamide, temperature-controlled reaction; the end point was detected by TLC, and the reaction ended in 1.5h; hot 5% NaOH solution was added to the reaction system, kept at 80°C to 85°C and washed 3 times, and then After washing with water at low temperature for 3 times, the reaction mixture was poured into cold water while it was hot, cooled, filtered, and dried to obtain 17.95 g of Intermediate I with a yield of 92.2% and a purity of 99.83%.
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