Furtrethonium iodide pharmaceutical intermediate 2- dimethylamino-methylfuran synthesis method

摘要

#$%^&*AU2016102309A420170223.pdf#####ABSTRACT Furtrethonium iodide pharmaceutical intermediate 2dimethylamino-methylfuran synthesis method, comprising the following steps: equipped with a stirrer, a thermometer and a dropping funnel , the reaction vessel was added 1.6mol dimethylamine methanol solution (3), 500ml oxalic acid solution, 1.8 mol alumina, 2.1-2.6mol 2-furan dimethanol solution (2), controlling the stirring speed 130-170rpm, raised the solution temperature to 120-128 0C, continued the reaction for 5-8h, reducing the temperature of the solution to 90--96 0C, refluxed for 2-3h, added 130ml phosphoric acid solution after cooling, increased solution temperature to 60--66 0C, stirred for 90-130 min, added 300ml sodium sulfite solution, continued reaction for 80-110min, the temperature of the solution is reduced to 10 - 15 0C, added 1 10ml potassium hydrogen sulfite solution, allowed to stand for 3-5h, the solution appeared layer, separated the oil, the aqueous layer was extracted for 5-8 times with nitromethane solution, combined oil layer, dehydrated with dehydration agent, vacuum distillation, collecting fractions of 110--116 0C, recrystallized from toluene solution, got 2- dimethylamino-methylfuran .