合成乙酰水杨酸的反应条件的探讨

对乙酰水杨酸"老药新用"的应用现状以及应用前景进行了详细的分析。比较了目前市场上乙酰水杨酸各种合成方法的优劣,设计了适合于工业化的较佳的合成路线,考察了原料物质的量之比、催化剂用量、反应温度、反应时间对反应收率的影响,进一步优化了合成工艺。经过实验数据的处理与分析,采用O-酰基化反应合成乙酰水杨酸的适宜条件为:无水环境下,对甲苯磺酸为催化剂,n(水杨酸)∶n(乙酸酐)=1∶2.0;反应温度为85℃和反应时间为30 min时,乙酰水杨酸的收率高于97%。所得样品符合《中国药典》和《美国药典》中乙酰水杨酸的质量要求,能够用于合成乙酰水杨酸。

Research of Reaction Conditions about Acetylsalicylic Acid Synthesized

Acetylsalicylic acid ＂new use for an old drug＂ application status and application prospect were analyzed in detail. Compared with the present market of acetylsalicylic acid synthesis methods advantages and disadvantages. Design suitable for industrialization of better synthetic route. The effect of raw material ratio, the dosage of catalyst, reaction temperature, reaction time on the yield of the reaction, further optimization of the synthesis technology. Through the experimental data processing and analysis, the O acylation reaction conditions for synthesis of acetyl salicylic acid： without water environment, concentrated 4-Toluene sulfonic acid as catalyst, n（salicylic acid） ＂ n（acetic anhydride）=l ： 2.0; when the reaction temperature of 85 ℃ and reaction time of 30 min, acetyl salicylic acid yield were higher than 97 %. The sample meets acetylsalicylic acid quality requirements of＂Chinese Pharmacopoeia＂ and ＂with the United States Pharmacopoeia＂, can be used for the synthesis of acetyl salicylic acid.