#$%^&*AU2016102269A420170223.pdf#####ABSTRACT Miconazole drug intermediates a- (2,4- dichlorophenyl) -aX- (1imidazolyl) ethanol synthesis method , comprising the following steps: (i) equipped with a stirrer, the reaction vessel was added 210ml cyclohexane solution, 0.11mol 2,4, w - trichloro acetophenone (2), controlling the stirring speed 140-170rpm, added 0.16-0.18mol lithium aluminum hydride tri-tert, controlled addition time in 2-3h, the solution temperature is raised to 40-45 C, continued the reaction for 30-36 h, cyclohexane was distilled off under reduced pressure, 160ml acetonitrile solution was added, atmospheric distillation, until the solvent evaporated to dryness, got the intermediate (3); (ii) a separate reaction vessel was added 160ml nitromethane solution, added 0.23 mol cuprous chloride, after all cuprous chloride was dissolved, the solution temperature is raised to 45 - 50 C, added 0.14- 0.16mol imidazole amine, continued the reaction for 3-4h, nitromethane was distilled off under reduced pressure, 160ml toluene solution was added, the solution temperature is raised to 90--100 C, added dropwise intermediate (3) , controlled adding time in 2-3h, controlled stirring speed 150-170rpm, continued the reaction 2h, the solvent toluene was removed under reduced pressure, cooled, poured into 1.2L potassium chloride solution , the temperature of the solution is reduced to 3 - 5 C, theprecipitated solid was suction filtered, washed with saline solution, dehydrated with dehydrating agent, recrystallized in nitroethane solution , got crystals a- (2,4- dichlorophenyl) -ax- (1- imidazolyl) ethanol.
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