Urapidil drug intermediates 1,3-dimethyl-6- (3-hydroxypropyl) amino uracil synthesis method

摘要

#$%^&*AU2016102286A420170223.pdf#####ABSTRACT Urapidil drug intermediates 1,3-dimethyl-6- (3-hydroxypropyl) amino uracil synthesis method , comprising the following steps: equipped with a stirrer, thermometer and reflux condenser, the reaction vessel was added 0.61mol 1,3-dimethyl-6-hydroxy-uracil (2), 0.72-0.75 mol 3- amino-1-propanol, 0.16mol sodium sulfite solution, controlling the stirring speed 130-160rpm, raised the solution temperature to 150-160 C, continued the reaction for 90-120min, reducing the temperature of the solution to 60-65 C, 230ml cyclohexane solution, refluxed for 30-50min, filter and the filtrate temperature was reduced to 5--9 C, allowed to stand for 30-35h, precipitated crystals by filtration, the resulting crystals were successively washed with saline solution, washed with acetonitrile solution, dehydrated with dehydrating agent, and recrystallized from isopropanol solution, got white crystals of 1,3-dimethyl-6(3-hydroxypropyl) amino uracil .