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合成一种具有生物活性的水苏碱衍生物。在氩气保护,0℃反应条件下进行反应,将二氯亚砜缓慢加入盛有水苏碱的圆底烧瓶中搅拌反应,5 min后将苄醇或β-苯乙醇加入反应体系,0℃剧烈搅拌1 h后升至室温继续反应48 h,TLC检测反应进程。反应完毕后加入200 m L乙醚稀释反应体系出现大量白色固体产生,减压抽滤得白色固体产品,真空干燥箱干燥得纯品。通过对酯化反应中会使用到的缩合剂(如DCC、DIC、EDC·HCl等)、二氯亚砜用量(1.2,2.0,3.0,4.0 Equiv)以及反应时间(12,24,48,60 h)进行详细考察得出其中缩合剂对反应没影响,确立最优反应条件是在氩气保护,0℃下,二氯亚砜的用量为3 Equiv反应48 h,成功合成目标产物,所得化合物结构的正确性经1H NMR、13C NMR和MS确认。
Synthesis of a bioactive stachydrine derivative. The reaction was carried out under the protection of argon at 0 ° C. Thionyl chloride was slowly added into a round-bottom flask containing stachydrine and stirred for reaction. After 5 min, benzyl alcohol or β-phenylethanol was added to the reaction system at 0 ° C Stirring was continued for 1 h and then to room temperature for 48 h. The reaction was monitored by TLC. After the reaction was completed, a large amount of white solid was produced by diluting the reaction system with 200 mL of ether. The white solid product was filtered under reduced pressure and vacuum dried to obtain a pure product. By using the condensing agent (such as DCC, DIC, EDC · HCl, etc.) which will be used in the esterification reaction, the amount of thionyl chloride (1.2,2.0,3.0,4.0 Equiv) and the reaction time (12,24,48,60 h) to obtain a detailed examination of which the condensing agent had no effect on the reaction. The optimum reaction conditions were as follows: the target product was successfully synthesized under the protection of argon at 0 ° C for 48 h. The correctness of the structure was confirmed by 1H NMR, 13C NMR and MS.