【摘要】 制备了对甲苯磺酸铜,替代腐蚀性强、副反应多的质子酸作为催化剂,用于催化甘油和苯甲醛缩合反应。利用响应面分析法对工艺条件进行了优化,得出最佳工艺条件为:n(甘油)/n(苯甲醛)=1.3,V(石油醚)/V(苯甲醛)=1.3,催化剂用量为苯甲醛物质的量的0.9%,缩醛收率为96.0%。该缩醛是两种物质的同分异构体混合物,考察了两种物质间的转化条件,并以甲苯为溶剂,在-20℃下,通过结晶法大量分离出了高价值的顺式六元环,收率40.8%,纯度为96.8%。探讨了相关反应机理,并利用GC-MS、IR和1HNMR对产物进行定量和定性分析。更多还原

【Abstract】 Copper p-toluenesulfonate was prepared for replacing the bronsted acid which has strong causticity and many side effects. It can be employed as the catalyst for the condensation of glycerol with benzaldehyde and good results were obtained. By optimizing the process with response surface methodology,the concrete procedure was as follows. The molar ratio of benzaldehyde to glycerol was1∶1. 3,the volume for petroleum ether was 1. 3 times of benzaldehyde and the dosage of catalyst was0. 9% of benzaldehyde. The yield of benzaldehyde glycerol acetal showed the maximum conversion of96. 0%. The acetal was an isomer mixture of two kinds of substance. The transformation conditions between isomers by taking toluene as solvent were investigated. The high value of cis six-member ring was isolatedextensively by crystallization under low temperature( about- 20 ℃). The yield of the product was 40. 8% and its purity was 96. 8%. The reaction mechanism was explored. Furthermore,the characterization of the target products were analyzed by means of GM-MS,IR and1 HNMR.更多还原