Dyphylline pharmaceutical drug 7- (2,3-dihydroxypropyl) – theophylline synthesis method

摘要

#$%^&*AU2016102264A420170223.pdf#####ABSTRACT Dyphylline pharmaceutical drug 7- (2,3-dihydroxypropyl) theophylline synthesis method , comprising the following steps: quipped with a stiffer, a reflux condenser, a dropping funnel and a thermometer, the reaction vessel was added 300ml potassium hydrogen sulfite solution, 0.71 mol stannous chloride, controlling the stirring speed 130-160rpm, raised the solution temperature to 60--65 C, slowly added 0.56mol theophylline (2), raised the solution temperature to 80 - 85 C, controlled the reaction 90-120min, the temperature of the solution is reduced to 50--55 C, dropped dropwise 1.2-1.4mol 3-amine 1,2 - propylene glycol (3), continued the reaction 120-160min, increased the solution temperature to 130-140 C , continued reaction for 60-70min, vacuum distillation, after removal of water, cooled, hexane solution was added heated to reflux, the condensation completely dissolved, filtered while hot, washed the filter cake with ethyl acetate, washed solid , cooled, suction filtered, washed with salt solution, washed with acetonitrile solution and recrystallized from nitromethane solution, got crystals of 7(2,3 -dihydroxypropyl) - theophylline .