【摘要】 以截短侧耳素、对甲苯磺酰氯和二甲基半胱胺盐酸盐为主要原料,以乙醚为溶剂,采用一锅法合成沃尼妙林中间体14-O-[(2-氨基-1,1-二甲基乙基)硫甲羰基]目特林。最佳工艺条件为:n(截短侧耳素)∶n(对甲苯磺酰氯)∶n(二甲基半胱胺盐酸盐)=1∶1.1∶1.1;相转移催化剂为四丁基溴化铵,用量为1.6 g;反应温度为30℃;反应时间为2.5 h;目标产物收率达91%。并用正交设计法对主要工艺条件进行了优化,结果与单因素实验结果相同。产品结构通过核磁共振波谱、红外光谱进行了表征,测定了产物的熔点。更多还原

【Abstract】 Valnemulin intermediate,14-O-[(2-amino-1,1-dimethylethyl)thiomethylcarbonyl]mutilin,was prepared by one-pot method with pleuromutilin,4-toluenesulfonyl chloride and dimethylcysteamine hydrochloride in diethyl ether.The optimum conditions were ascertained as follows:n(pleuromutilin)∶ n(4-toluene sulfonyl chloride)∶ n(dimethyl cysteamine hydrochloride)=1∶ 1.1∶ 1.1,tetrabutyl ammonium bromide being used as phase transfer catalyst,the amount of tetrabutyl ammonium bromide being 1.6 g,reaction time 2.5 h,reaction temperature 30 ℃;under such optimum conditions,the yield of the product was 91%.An orthogonal design incorporating 4 factors at 3 levels was applied to optimize the main process conditions,the results of which were in accordance with the single factor experimental data.The structure of the target compound was characterized by means of 1HNMR,IR and its melting point was measured.更多还原