摘要:
目的 改进他米巴罗汀的合成工艺.方法 以2,5-二甲基-2,5-己二醇为起始原料经氯代后与乙酰苯胺进行Friedel-Crafts环合反应制得1,2,3,4-四氢-1,1,4,4-四甲基-6-乙酰氨基萘,再经脱乙酰基、酰化、水解共5步反应合成了抗白血病药物他米巴罗汀.结果 优化后的工艺成本低、后处理容易、产物纯度高(纯度>99.7%,单个杂质<0.1%)、收率高.结论 新工艺的总收率达到26.6%,且适合工业化生产.目标产物结构经1H-NMR,ESI-MS和元素分析确证.
Abstract:
Objective To improve the preparation process of tamibarotene.Methods 1,2,3,4-tetrahydro-1,1,4,4-tetram-ethyl-6-acelylaminonaphthalimide was prepared from 2,5-dimethyl-2,5-hexanediol by chloridized and Friedel-Craft reaction with acetauilide,which was subjected to deacylation, acylation and hydrolyzation to give tamibarotene.Results The process was successfully improved due to low cost,easier post-processing and good yield. The purity of the product was high (>99.7%) and no impurity more than 0.1%. Conclusion The total yield of the improved process was 26.6%. which was more suitable for industrial manufacturing.the structure of temibarotene was confirmed by 1H-NMR,ESl-MS and elementary analysis.
点击查看大图
下载:
