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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。
Objective To improve the synthesis of tamibarrine. Methods 2,5-Dimethyl-2,5-hexanediol was used as the starting material to carry out the Friedel-Crafts cyclization reaction with acetanilide after chlorination to obtain 1,2,3,4-tetrahydro-1, 1,4,4-tetramethyl-6-acetamidonaphthalene, followed by deacetylation, acylation, hydrolysis a total of five steps reaction lemiferaide drug Tamibarotene. Results The optimized process cost was low, post-treatment was easy, the product purity was high (purity> 99.7%, single impurity <0.1%), and the yield was high. Conclusion The total yield of new technology reached 26.6%, and suitable for industrial production. The structure of the target product was confirmed by1H-NMR, ESI-MS and elemental analysis.