顺-2-苯基-1,3-二噁烷-5-醇的合成工艺优化及提纯研究

Optimization of the synthesis of cis-2-Phenyl-1,3-dioxan-5-ol and study on purification

摘要:

制备了对甲苯磺酸铜，用它取代腐蚀性强、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，取得了较为满意的结果。利用响应面分析法对合成工艺进行了优化，得出最佳工艺：甘油比苯甲醛为1.3（摩尔比），石油醚体积用量为苯甲醛的1.3倍，催化剂用量为苯甲醛的0.9mol%，缩醛最大收率为96.0%。该缩醛是2种物质的同分异构体混合物，考察了2种物质间的转化条件，并利用甲苯为溶剂，在-20℃的低温条件下，通过结晶法大规模的分离出了高价值的顺式六元环，纯度为96.8%，分离选择性为40.8%。探讨了相关反应机理，利用GC-MS、IR和1HNMR对产品进行定量和定性分析。

Abstract:

Copper p-toluenesulfonate was prepared for replacing the Bronsted acid, which has a strong corrosive and many side effects. It can be employed as the catalyst for the condensation of glycerol with benzaldehyde and reached a good result. By optimizing the process with response surface methodology, the concrete procedure was as follows. The molar ratio of benzaldehyde to glycerol was 1:1.3, the volume for petroleum ether was 1.3 times of benzaldehyde and the dosage of catalyst was 0.9mol% of benzaldehyde. The yield of benzaldehyde glycerol acetal showed the maximum conversion of 96.0%. The acetal was an isomer mixture of two kinds of substance. It observed the transformation conditions between isomers by taking toluene as solvent. The high value of cis six-member ring was separated out extensively by crystallization under low temperature (about -20°C). The purity of the product was 96.8% and isolated selectivity was 40.8%. The reaction mechanism was explored. Furthermore, the characterization of target products were analyzed by means of GM-MS,IR and 1HNMR．