| 摘要 |
Terbinafine drug intermediates tert-butylacetylene synthesis method, comprising the following steps: equipped with a stiffer, a thermometer, a dropping funnel, a condenser, the reaction vessel was added 310ml potassium bisulfate solution, 300ml hexane solution, the solution temperature was raised to 90--95 C, stirring speed was controlled at 150-170rpm, 0.73mol 1,1-diamino-3,3-dimethylbutane(2) was added dropwise, the addition time was controlled within 3-5h, 0.81-0.84mol hypochlorous acid benzyl ester (3) was added, reacted for 90-120min, the solution temperature was raised to 110--115 C , the reaction was continued for 3-5h, the temperature of the solution is reduced to 10-150C, the precipitated solid was filtered, washed with salt solution, washed with acetonitrile solution, vacuum distillation, collecting fractions 100--108 C, and recrystallized from cyclohexane solution, got crystals of tert-butylacetylene. |
