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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。
The title compound was synthesized from isobutyl aldehyde and 2,2,4-trimethyl-1,3-pentanediol (TMPD). The catalytic properties of different molecular sieves were investigated, Hβ zeolite with the best activity was used as catalyst. The effect of catalyst dosage, reaction time, aldol ratio and water-entraining agent on the reaction and the recycle of catalyst were investigated. The results showed that 30.0 mmol of isobutyl aldehyde and 10.0 mmol of TMPD with toluene as the water-carrying agent under the optimal conditions were 0.20 g of catalyst and 2.0 h of refluxing solvent, yield of 95.1% . Hβ zeolite also has good reusability of the molecular sieve, after 6 repeated use remained high activity. In addition, the reaction of TMPD with other aldehydes and ketones was also investigated using Hβ zeolite as catalyst. The catalytic activity of TMPD was similar to that of other aldehydes and ketones. The yield of the corresponding alkanes was above 90%.