摘要
采用星点设计-效应面优化法对2-金刚烷基乙醛酸5合成2-(3-羟基-1-金刚烷基)-2-乙醛酸6的因素进行考证,以提高化合物6的收率。以金刚烷甲酸1为起始原料,酰氯化后与丙二酸二乙酯钠盐缩合,脱羧得到乙酰金刚烷4,4经两步高锰酸钾氧化分别得5和6。化合物5到6的氧化反应是关键步骤,通过单因素考察法对化合物5合成6的工艺影响因素进行初步考察,并用星点设计-效应面优化法对显著性因素进行优化和多元线性回归与二项式方程拟合。优化后的化合物4到6的工艺总收率由文献报道的30%～40%提高到57.8%。星点设计-效应面优化法是一种简便、可行的工艺优化方法。
To improve the yield of the compound 6, the method of central composite design-response surface methodology was used to 2-adamantyl glyoxylic acid 5 synthesis 2-（3-hydroxy-l-adamantyl）-2-oxoacetie acid 6. The 5 and 6 was synthesized from adaman- tane formic acid 1 via reaction with dimethyl sulfoxide, diethyl malonate sodium salt and decarboxylation to give acetyl adamantine 4 which was subjected to two step oxidation by potassium permanganate. Because of the process 5 to 6 was a key step, the significant factors method was preliminary utilized to synthesis compound 6 and the central composite design-response surface methodology was to optimize the significant factors and multiple linear regression and binomial equation fitting. Finally, the total yield of 4 to 6 was reached 57.8% from 30%～40%. Central composite design-response surface methodology was a feasible and convenient method.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2013年第2期194-199,共6页
Chemical Research and Application
基金
重庆市自然科学基金项目(2006BB5286)资助
重庆医科大学大学生科学研究与创新实验资助项目(201224)资助
