1,4-二氧杂螺[4.5]癸烷-8-酮的合成Synthesis of 1,4-Dioxaspira[4.5]decan-8-one
晋平,刘亮,张国亮,张凤宝
摘要(Abstract)：
以1,4,9,12-四氧杂二螺[4.2.4.2]十四烷为原料,采用酸性条件下水解缩酮选择性地脱除单侧羰基保护的方法合成了1,4-二氧杂螺[4.5]癸烷-8-酮。通过对盐酸、硫酸、甲酸、醋酸等催化性能的比较,对选择性的机理和影响因素进行了探讨,确定醋酸作为催化剂。优化了反应工艺条件,并对产品进行了IR、1HNMR的确认。结果表明,以冰醋酸作催化剂,反应溶剂V(冰醋酸):V(H2O)=5:1,反应浓度为0.05g?mL?1,反应温度为65℃时,与原方法相比,反应时间由15h缩短为约11min,产物的色谱收率由65%提高到80%。
关键词(KeyWords)： 1,4-二氧杂螺[4.5]癸烷-8-酮;1,4,9,12-四氧杂二螺[4.2.4.2]十四烷;选择性去保护;水解
基金项目(Foundation):
作者(Author): 晋平,刘亮,张国亮,张凤宝
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