摘要
实验以丁二酸酐和邻苯二甲醚为原料,研究了以无水氯化铝作为催化剂,硝基苯作为溶剂,通过Friedel-Crafts酰基化反应制备3-(3,4-二甲氧基苯甲酰基)丙酸,探讨了原料摩尔比、催化剂用量、反应时间和反应温度4个因素对3-(3,4-二甲氧基苯甲酰基)丙酸产率的影响,并在单因素实验的基础上通过Boxbenhnken实验设计和响应面分析得出3-(3,4-二甲氧基苯甲酰基)丙酸的最佳合成工艺条件为:反应体系中邻苯二甲醚添加量为20mmol时,丁二酸酐与邻苯二甲醚摩尔比1.2∶1,催化剂无水Al Cl3用量6.56g,反应时间8.2h,反应温度61℃,此条件下3-(3,4-二甲氧基苯甲酰基)丙酸产率可达到88.73%。
In this research, 3-（3, 4-Dimethoxybenzoyl） propionic acid was prepared through Friedel-Crafts acylation reaction between succinic anhydride and veratrole with aluminiumtrichloride as the catalyst and nitrobenzene as the solvent. The effects of raw material ratio, catalyst dosage, reaction time and reaction temperature on the yield of the target product were investigated. The optimum conditions of 3-（3, 4-Dimethoxybenzoyl） propionic acid synthesis were determined by the single factor test and the response surface methodology and the optimal parameters were ： veratrole 20mmol, the ratio ofsuccinic anhydride and veratrole 1.2 ： 1, catalyst dosage 6.56g, reaction time 8.2h, reaction temperature 61℃. Under the conditions above, the yield of 3-（3, 4-Dimethoxybenzoyl） propionic acid was 88.73%.
出处
《中国食品添加剂》
CAS
北大核心
2015年第4期154-160,共7页
China Food Additives
