Miconazole drug intermediates 2,4 - dichlorophenyl chloromethyl ketone synthesis method

摘要

#$%^&*AU2016102167A420170216.pdf#####ABSTRACT Miconazole drug intermediates 2,4 - dichlorophenyl chloromethyl ketone synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a reflux condenser, a dropping funnel, the reaction vessel was added 0.4mol dichlorobenzene (2), 0.53-0.55mol stannous chloride, controlling the stirring speed at 150-170rpm, 0.46-0.48mol was slowly added chloroacetamide, addition time was controlled within 80-90min, the solution temperature is raised to 60--65 C, the reaction time was controlled within 4-5h, the reaction was poured into 900ml potassium chloride solution, the temperature of the solution is reduced to 5 --7 C, the precipitated pale yellow solid was filtered, washed with saline solution, recrystallized from hexane solution, decolorized with zeolite, the temperature of the solution is reduced to 3--4 C, yellow flake crystals precipitated, suction filtered, washed with methyl amine solution, dehydrated with dehydrating agent, got 2,4 - dichlorophenyl chloromethyl ketone.