2,2-二羟甲基丁醛的催化合成与表征

采用新制的正丁醛（NBAL）和多聚甲醛（PFA）在三乙胺（TEA）催化下制备了合成三羟甲基丙烷（TMP）的中间产物2,2-二羟甲基丁醛（DMB）.探讨了原料配比和反应时间对DMB收率的影响，以及催化剂与含水量对反应体系升温速率及DMB收率的影响.最佳工艺条件为：N₂保护下，n_NBAL∶n_PFA∶n_TEA为1∶3∶（0.05～0.1），含水量为10％～15％（以总量计），反应温度为50～80℃，反应时间为2h.通过IR、GC、GC-MS、¹HNMR对DMB的结构进行了表征；经过GC分析，NBAL在上述条件下可反应完全（＞99％），DMB收率达88％以上.

CATALYZED SYNTHESIS AND CHARACTERIZATION OF 2,2-DIMETHYLOL-1-BUTANAL

2,2-dimethylol-1-butanal(DMB) was synthesized by n-butyraldehyde（NBAL）with paraformaldehyde（PFA）in the existence of triethylamine（TEA）. NBAL reacted completely(＞99％) and the yield of DMB reached 88%.The structure of DMB was characterized by IR、GC、GC-MS、¹HNMR.It was found that the concentration of TEA and H₂O greatly affected the rate of temperature rise of the reaction system and the yield of DMB. The optimized reaction conditions were as follows:under the nitrogen atmosphere,n_NBAL∶n_PFA∶n_TEA=1∶3∶(0.05—0.1)and 10%—15% water by weight, temperature 50—80℃,reaction time 2h.