944555五氟戊基巯基壬基1醇的合成研究.pdfVIP

9-(4,4,5,5,5-五氟戊基巯基)壬基-1-醇的合成 1 1 1∗ 2 1 王曾华 , 李运波 , 孟春 , 赵学清 ，郭养浩 （1 福州大学化学化工学院，福建 福州350108 ；2 福建省微生物研究所，福建 福州350007 ） 摘要: 9-(4,4,5,5,5-五氟戊基巯基) 壬基-1-醇是治疗晚期乳腺癌新药氟维司群的重要有机中间体，以 4,4,5,5,5-五氟-1-戊醇对甲苯磺酸酯和 S-9-羟基壬基异硫脲为原料合成 9- （4,4,5,5,5-五氟戊基巯基）壬 基-1-醇目标产物，通过实验优化合成路线，确定了最优反应条件。结果表明：该反应以丙酮：水(5 ： 1)为溶剂，以氢氧化钠为催化剂，加热回流18 h，收率可达84.8%。利用IR 、MS 、 1HNMR 等方法 对产物进行了结构表征。 关键词：9-(4,4,5,5,5-五氟戊基巯基)壬基-1-醇；S-9-羟基壬基异硫脲；合成 中图分类号：O 62912 文献标识码：A 文章编号： Synthesis of 9-(4,4,5,5,5-pentalfluropentylmercapto)nonyl-1-alcohol 1 1 1 2 WANG Zenghua , LI Yunbo , MNEG Chen , ZHAO Xueqing 1 ( Chemistry and Engineer institute, Fuzhou University, Fuzhou 350108, fujian, China; 2 Fujian Institute of Microbiology, Fuzhou 350007, fujian, China) Abstract: The process of preparing 9-(4,4,5,5,5-pentalfluropentylmercapto)nonyl-1-alcohol ，as one of the important intermediates in the therapy of Fulvestrant-a new drug for advanced breast cancer for synthesis was studied ，the title compound was prepared from 4,4,5,5,5-pentalfluro-1- pentanol Pmethylbenzensulfonate and S-9-hydroxynonyl isothiourea.The influences of reaction conditions on the yield were investigated ，the optimal reaction conditions were as follows : acetone : water (5 : 1) as dissolvent ，sodium hydrate as catalyst，heating circumfluence for 18h and 1 yield was 84.4%. The product was characterized with IR ，MS ，HNMR analysis. Key words ：9-(4,4,5,5,5-pentalfluropentylmercapto)nonyl-1-alcohol；S-9-hydroxynonyl isothiourea ；synthsis ∗联系人：孟春. 第一作者：王曾华 （1983-），