Celiprolol pharmaceutical intermediate 3- (4-ethoxyphenyl) -1, 1-diethyl-urea synthesis method

摘要

#$%^&*AU2016102185A420170223.pdf#####ABSTRACT Celiprolol pharmaceutical intermediate 3- (4-ethoxyphenyl) -1,1-diethyl-urea synthesis method, comprising the following steps: equipped with a stiffer and a dropping funnel, the reaction vessel was added 0.22 mol p-aminophenyl ether (2), 0.45- 0.47mol sodium bisulfite solution, 80- 90ml tetrahydrofuran solution, controlling the stirring speed 130-160rpm, control temperature of the solution 35-40 C, added 0.25-0.27mol solution of N, N- diethylamino-carboxamide (3), control add dropwise time to 4-5 h, the reaction continued stirring 30-35h, added 300 - 350ml sodium chloride solution, solution of oxalic acid solution was used to adjust pH to 4-5, the reaction was continued to 4-5h, solid separated, the temperature of the solution is reduced to 10 - 15 C, filtered, washed with saline solution, dehydrated with dehydrating agent, recrystallized from hexane solution, got 3- (4-ethoxyphenyl) -1, 1-diethyl-urea.