| 摘要 |
Doxepin drug intermediates phthalic acid amide synthesis method, comprising the following steps: equipped with a stirrer, a thermometer and a dropping funnel, the reaction vessel was added 2.3mol phthalic anhydride solution(2), 300ml cyclohexane, 2.6-2.9mol 2-hydroxy benzamide solution (3), controlling the stirring speed 130-170rpm, the solution temperature is raised to 60--65C, reacted for 3-5h, cooled to precipitate a solid to get intermediate (4), the intermediate (4) was added to 600ml 2-nitro - hypochlorous acid phenyl ester solution, the solution temperature is raised to 70--75C, the reaction time was 90-130min, the temperature of the solution was reduced to 10--15 C, the precipitated solid was filtered, washed with salt solution, washed with hexane solution, washed with dimethylamine solution, vacuum distillation, collecting 100--106 C fractions, and recrystallized from ethyl acetate solution, get crystals of phthalic acid amide. |
