考察了原料投料比、不同溶剂、碱性试剂及反应时间等条件对反应收率的影响，对乙酰香兰素合成工艺优化及反应进程进行了研究。实验以香兰素和乙酸酐为原料，反应合成乙酰香兰素。采用毛细管熔点法、傅里叶变换红外光谱（FT-IR）及气相色谱-质谱/质谱（GC-MS/MS）对乙酰香兰素反应进行分析和表征。实验结果表明，乙酰香兰素的合成工艺优化条件为原料摩尔比n（香兰素）:n（乙酸酐）:n（三乙胺）=1:1.3:0.5，室温反应0.5 h，收率可达99.0%。初步探讨了碱性试剂三乙胺作为催化剂在反应进程当中所起的催化作用，并对其反应机理进行了推测。该工艺反应条件温和，反应时间短，收率高，原料价廉易得，操作简单易行。乙酰香兰素反应进程的研究为合成工艺优化、分析检测方法及基础理论研究提供了一定的参考依据。
Acetylvanillin （4-acyloxy-3-methoxy-benzaldehyde） is an important vanillin derivative, which has strong milk fragrance. It is an intermediate produced in the reaction process of synthesizing vanillin from eugenol, isoeugenol and other raw materials. It is often used as flavoring agent in various dairy products （such as modulated milk powder, fresh milk, yogurt, etc.）, biscuits, beverages, cosmetics （perfume）, tobacco, wine, food packaging, feed, etc. Due to the structural characteristics of various functional groups （-CHO, AcO-, MeO-） on the benzene ring of acetylvanillin, it can undergo a variety of chemical reactions. Therefore, it is also widely used in the preparation of drugs and other fine chemicals as an important organic intermediate. At present, the chemical synthesis of acetylvanillin mainly takes vanillin as raw material, and it is prepared by acylation reagents such as anhydride and acyl chloride at room temperature following strong alkali or catalyst. However, this process has some shortcomings, such as incomplete reaction, long time of esterification, complicated post-treatment, corrosion in equipment, and difficult access to catalyst. In this work, the effects of experimental conditions on the yield were investigated, including the ratios of raw materials, the solvents, alkaline reagents and reaction time, and the optimization of synthesis process and the analysis of reaction process were carried out. Vanillin and acetic anhydride were used as raw materials. The reaction process of acetylvanillin was analyzed and characterized by capillary melting point method, FT-IR and GC-MS/MS. The results showed that, the optimized synthesis conditions of acetylvanillin were as follows. The molar ratio of raw materials n（vanillin） : n（acetic anhydride） : n（triethylamine） was 1:1.3:0.5; the reaction time at room temperature was 0.5 h, and the yield was 99.0%. The catalytic effect of triethylamine as the catalyst in the reaction process was discussed, and its catalytic mechanism was speculated. This process had the advantages of mild reaction conditions, short reaction time, high yield, low cost and easy availability of raw materials, and simple operation. This study could provide reference for the optimization of synthesis process, analysis method and basic theoretical research.
