摘要
本文报道4-溴-6-氯-1-{[2-(三甲基硅基)乙氧基]甲基}-1H-吡咯并[2,3-b]吡啶的合成方法及工艺。以4-溴-6-氯-1H-吡咯并[2,3-b]吡啶为原料,在Na H作用下,与氯甲基三甲基硅乙基醚(SEM-Cl)发生N-烷基化反应得到目标化合物。产物结构经过~1H NMR和ESI-MS表征。合成工艺研究发现,4-溴-6-氯-1-{[2-(三甲基硅基)乙氧基]甲基}-1H-吡咯并[2,3-b]吡啶(1)的适宜合成条件为:物料比为n(SEM-Cl))∶n(化合物2))=1.3∶1;NaH用量为n(NaH))∶n(化合物2))=1.1∶1;25℃反应2h,在该条件下产物收率78.5%。
The synthesis of 4-bromo-6-chloro-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrrolo[2,3-b]pyridine was reported.The target compound was synthesized by N-alkylation of 4-bromo-6-chloro-1H-pyrrolo[2,3-b]pyridine with:2-chloromethyl 2-(trimethylsilyl)ethyl ether(SEM-Cl)in the presence of sodium hydride.The structure of the product was characterized by~1H NMR and ESI-MS.The reaction conditions were investigated,and the suitable conditions for the N-alkylation reaction were determined as follows:material Ratio n∶n=1.3∶1;amount of sodium hydride n∶n=1.1∶1;the reaction was at 25℃for 2h.Under the reaction conditions,the yield of product was up to 78.5%.
作者
徐小娜
张婧
王晓霞
仝红娟
朱周静
XU Xiao-na;ZHANG Jing;WANG Xiao-xia;TONG Hong-juan;ZHU Zhou-jing(School of Pharmaceutical&Chemical Engineering,Xianyang Vocational Technical College,Xianyang 712000,China;Xianyang Key Laboratory of Molecular Imaging and Drug Synthesis,School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China)
出处
《化学工程师》
CAS
2022年第11期11-13,57,共4页
Chemical Engineer
基金
陕西省自然科学基础研究计划(面上)项目(2022JM-561)
咸阳职业技术学院博士科研基金项目(2021BK01)
陕西国际商贸学院“中药药效物质研究”创新团队资助项目(SSY18TD02)。
