微波促进SnCl4/C催化合成 2, 2-二羟甲基-1, 3-丙二醇双缩醛(酮)
来源期刊：中南大学学报(自然科学版)2006年第6期
论文作者：袁先友 张敏
文章页码：1137 - 1141
关键词：2, 2-二羟甲基-1, 3-丙二醇;缩酮;缩醛; SnCl4/C;微波
Key words：2, 2-bis(hydroxymethyl)-1, 3-propanediol; diacetal; diketal; SnCl4/C; microwave
摘 要：以活性炭负载SnCl4·5H2O为催化剂,利用微波技术合成8种2, 2-二羟甲基-1, 3-丙二醇双缩醛(酮),其中, 2, 2-二羟甲基-1, 3-丙二醇双缩辛醛属新化合物。采用元素分析、傅里叶转换红外光谱(FTIR)和氢核磁共振1H NMR对产物进行表征。以苯甲醛与2, 2-二羟甲基-1, 3-丙二醇的缩合为模型反应对工艺条件进行优化,得其优化反应条件为:催化剂负载量20%,催化剂用量0.25 g, 2, 2-二羟甲基-1, 3-丙二醇4 g(30 mmol),苯甲醛66 mmol,微波功率600 W,辐射时间1.5 min,产率89.3%。
Abstract: Eight kinds of 2, 2-bis(hydroxymethyl)-1, 3-propanediol diacetals and diketal were synthesized through condensation reaction of 2, 2-bis(hydroxymethyl)-1, 3-propanediol with aldehydes and ketone catalyzed by SnCl4·5H2O supported on active carbon under microwave irradiation and characterized by element analysis, FTIR, and1HNMR. Among these products, diacetal of 2, 2-bis(hydroxymethyl)-1, 3-propanediol withn-octanal is a new compound. The reaction conditions were investigated. Under the optimum reaction conditions(catalyst loaded amount 20%, catalyst amount 0.25 g, 2, 2-bis(hydroxymethyl)-1, 3-propanediol 30 mmol, benzaldehyde 66 mmol, microwave power 600 W, irradiation time 3min), the yield of diacetal reaches 89.3%.
