碳酸二甲酯作甲基化试剂合成丁香酚甲醚

摘要

Methyleugenol was prepared from eugenol in the presence of potassium carbonate (K2CO3) , using dimethyl carbonate (DMC) as methylating agent instead of the conventional toxic agents. Using the yield of methyleugenol as the evalution index, central composite design process was used to optimize the methylation reaction of eugenol and DMC. An optimum reaction condition for the preparation of the targeted product was as follows, reaction temperature 155℃ , the amount of K2CO36.12 % (measured by the molar ratio of eugenol) , the molar ratio of DMC and eugenol 4.3:1 and reaction time 6 h. Under this condition the conversion rate reached 96.16 %. Meanwhile, repeated experiments showed that the reaction process was easy to be controlled and excellent repetitiveness can be acquired. GC-MS and IR spectral analysis were employed to confirm the structure of the product.%以绿色化学原料碳酸二甲酯(DMC)代替传统有毒有害试剂作为甲基化试剂,以丁香酚为原料,在固体碱K2CO3催化作用下合成丁香酚甲醚.对几种不同催化剂进行筛选,确定K2CO3为催化剂；以丁香酚甲醚得率为评价指标,采用中心复合设计法对丁香酚和DMC甲基化反应的工艺进行优化,得到制备丁香酚甲醚的最佳工艺:反应温度155℃,K2CO3用量6.12％(占丁香酚的摩尔分数),n(DMC)∶n(丁香酚)4.3∶1,反应时间6h,在此条件下丁香酚甲醚得率的预测值为96.44％.对最佳工艺进行验证实验,丁香酚甲醚得率为96.16％,表明中心复合设计预测性良好,实验重复性好.采用气质联用、红外光谱对产物进行分析.