Hβ分子筛催化合成5,5-二甲基-2,4-二异丙基-1,3-二氧噁烷及其他噁烷类化合物  

Synthesis of 5,5-dimethyl-2,4-diisopropyl-1,3-dioxane and acetalization catalysed by Hβ zeolite

作　　者：刘玲[1] 赵月昌[1] 梁学正[1] 程文萍[1] 王有菲[1] 杨建国[1] 

机构地区：[1]华东师范大学上海市绿色化学与化工过程绿色化重点实验室,上海200062

出　　处：《化学试剂》2008年第7期493-496,共4页Chemical Reagents

基　　金：国家科技支撑计划项目(2006BAE03B06);上海市科委国际科技合作项目(06SR07101);上海市重点学科建设项目(B409)

摘　　要：以异丁醛和2,2,4-三甲基-1,3-戊二醇(TMPD)为原料,合成了标题化合物(青叶噁烷),考察了不同分子筛的催化性能,筛选出催化活性最佳的Hβ沸石分子筛为催化剂;并考察了催化剂用量、反应时间、醛醇比、带水剂等因素对该反应的影响,以及催化剂的循环使用性。结果表明,在最优化的反应条件下,30.0 mmol异丁醛,10.0 mmol TMPD,以甲苯为带水剂,催化剂用量为0.20 g,在溶剂的回流温度下反应2.0 h,产物收率达95.1%。Hβ沸石分子筛还具有很好的循环使用性,在重复使用6次后仍保持高的活性。此外,还考察了以Hβ沸石分子筛为催化剂,TMPD与其他醛酮的缩合反应,同样取得很好的催化效果,相应的噁烷类化合物的收率在90%以上。5, 5-Dimethyl-2, 4-diisopropyl-1,3-dioxane was syn-thesized through isobutylaldehyde and 2, 2,4-trimethy-1 , 3-pentanediol （TMPD） catalyzed by different zeolites. Finally, Hβ zeolite was chosen as the catalyst because of its preferable catalytic power. Furthermore, under this condition, the effects of different amounts of catalyst, different reaction time, different mole ratios of reactants and solvents on the product yield were investigated. The results indicated that the yield of 5,5-dimethyl-2,4-diisopropyl- 1,3-dioxane reached 95.1% under optimum reaction condition （isobutyraldehyde concentration ： 30.0 mmol, TMPD concentra- tion：10.0 mmol,Hβ zeolite dosage：0.20 g,using toluene as the solvent at, the reflux temperature for 2.0 h）.The experimental results revealed that the catalyst could be recycled with high activity, and no obvious change in yield was observed for 6 recycling times. Moreover,The catalyst has been applied to catalyze the acetalization and ketalization reactions. The results showed that the catalyst was very efficient on the reaction process, and the yields of respective products were above 90%.

关 键 词：Hβ沸石分子筛 异丁醛 TMPD 5 5-二甲基-2 4-二异丙基-1 3-二氧嗯烷 缩醛(酮)化 

分 类 号：TQ224.4[化学工程—有机化工]