Synthetic method of perhexiline drug intermediate alpha-(2,2-diphenyl vinyl) pyridine
A technology of diphenylethylene and perhexiline, which is applied in the field of synthesis of α-pyridine, an intermediate of perhexiline, can solve problems such as myocardial ischemia aggravation, reduce intermediate links, reduce reaction temperature and reaction time , the effect of increasing the reaction yield
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example 1
[0010] In a reaction vessel equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel, add 1.56mol of 1,1-diphenyl-2-(α-pyridyl)ethylamine (2), with a mass fraction of 30% Phenyl hypochlorite solution (3) 1.81mol, nitromethane 300ml, control the stirring speed 150rpm, increase the solution temperature to 80°C, react for 3h, lower the solution temperature to 45°C, add a mass fraction of 20% potassium carbonate solution to adjust pH is 9, continue to stir for 5 hours, reduce the temperature of the solution to 10°C, precipitate solids, filter with suction, wash with ammonium nitrate solution, wash with 50% chlorobenzene, decolorize with molecular sieves, stir and reflux for 3 hours, dehydrate with anhydrous potassium carbonate, and Recrystallized in p-xylene with a mass fraction of 90%, to obtain 276.63 g of crystalline α-(2,2-diphenylvinyl)pyridine, with a yield of 69%.
example 2
[0012] In a reaction vessel equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel, add 1.56mol of 1,1-diphenyl-2-(α-pyridyl)ethylamine (2), with a mass fraction of 32% Phenyl hypochlorite solution (3) 1.9mol, nitromethane 300ml, control the stirring speed at 170rpm, raise the solution temperature to 82°C, react for 4h, lower the solution temperature to 47°C, add a mass fraction of 23% potassium carbonate solution to adjust The pH is 9, continue to stir for 6 hours, reduce the temperature of the solution to 12°C, precipitate solids, filter with suction, wash with potassium iodide solution, wash with 52% chlorobenzene, decolorize with molecular sieves, stir and reflux for 3 hours, dehydrate activated alumina, Recrystallized from 92% p-xylene to obtain 292.67 g of crystalline α-(2,2-diphenylvinyl)pyridine with a yield of 73%.
example 3
[0014] In a reaction vessel equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel, add 1.56mol of 1,1-diphenyl-2-(α-pyridyl)ethylamine (2), with a mass fraction of 35% Phenyl hypochlorite solution (3) 2.1mol, nitromethane 300ml, control the stirring speed at 190rpm, raise the solution temperature to 85°C, react for 5h, lower the solution temperature to 50°C, add a mass fraction of 25% potassium carbonate solution to adjust The pH is 10, continue to stir for 7 hours, lower the solution temperature to 15°C, precipitate solids, filter with suction, wash with ammonium nitrate solution, wash with 55% chlorobenzene, decolorize with molecular sieves, stir and reflux for 4 hours, dehydrate with anhydrous potassium carbonate, and Recrystallized in p-xylene with a mass fraction of 95%, to obtain 312.72 g of crystalline α-(2,2-diphenylvinyl)pyridine, with a yield of 78%.
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