以环酮和季戊四醇为原料,磷钨酸为催化剂,在甲苯中回流分水反应合成了系列氧杂三螺环化合物(3a-3h),其中5,9,14,17-四氧杂三螺E3.2.2.3^10.2^7.2^4]十七烷(3a)和7,11,18,21-四氧杂-3,15-二硫杂三螺[5.2.2.5^12.2^9.2^6]二十一烷(3f)为新化合物,其结构经^1H NMR,^13CNMR和HR—Ms(ESI)表征。并以3c的合成为模板反应,对反应条件进行了优化。
A series of oxatrispiro derivatives(3a - 3h) were prepared by reflux of pentaerythritol with cyclic ketones in toluene using phosphotungstic acid as the catalyst. Among them, 5,9,14,17-tetraox- atrispiro [ 3.2.2.310.27. 24] heptadecane (3a) and 7,11,18,21-tetraoxa-3,15-dithiatrispiro [ 5.2.2. 5^12 2.29. 26] henicosane(3f) were new compounds. The structures were characterized by 1H NMR, 13C NMR and HR-MS(ESI). The reaction conditions were optimized using synthesis of 3c as the template reaction.