| 摘要 |
Hexyl resorcinol drug intermediates 2-heptanone synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a dropping funnel, the reaction vessel was added 2.1L potassium bisulfite solution, 1.6mol n-butyl-propionamide solution, 1.9-2.3mol 2-nitro-hypochlorous acid phenyl ester solution, 330ml nitroethane solution, stirring speed was controlled at 130-170rpm, the solution temperature was raised to 60-65 C,reacted for 7-9h, the oil layer was separated, adding sodium sulfite, the solution was adjusted to pH 9-10, the reaction was continued for 30-50min, reduce the temperature of the solution to10-15 C, the precipitated solid was washed with salt solution, washed with ethyl acetate solution, dehydrated with dehydrating agent, vacuum distillation, collecting fractions of 90-95 C, recrystallized from p-xylene solution, got crystals of 2-heptanone. |
