摘要
以2-氨基-4-羟基-5-甲氧基苯甲酸甲酯(化合物2)和1-(3-羟丙基)四氢吡咯(化合物3)为原料,通过光延反应得到2-氨基-5-甲氧基-4-[3-(吡咯烷-1-基)丙氧基]苯胺(化合物1)。通过1H-NMR和ESI-MS对化合物1的结构进行了表征,并对反应条件进行了优化。确定的最佳的反应条件为:反应溶剂为四氢呋喃,n(化合物2)∶n(偶氮二甲酸二叔丁酯)∶n(化合物3)=1∶1.2∶2.0,n(三苯基膦)∶n(化合物2)=1∶1,反应时间为3h。在此反应条件下,化合物1的收率可达到65.4%。
The target compound 2-amino-5-methoxy-4-[3-(pyrrolidin-1-yl)propoxy] aniline(1) was synthesized from 2-amino-4-hydroxy-5-methoxybenzoate(2) and 1-(3-hydroxypropyl)-pyrolidine(3),The structures of the target compound 1 were characterized by 1H-NMR and ESI-MS and the reaction conditions were optimized.The research showed that the optimization conditions were terthydrofuran as sollvent, n(2) ∶n(Di-tert-butyl azodicarboxylate) ∶n(3)=1∶1.2∶2.0,n(triphenylphosphine)/n(2)=1∶1,reaction time was 3 h.The yield of the target compound 1 was 65.4% when the reaction was conducted under the optimization conditions.
作者
刘懿
吕莹莹
李改园
程越
蒋伟
高艳蓉
唐文强
LIU Yi;LYU Ying-ying;LI Gai-yuan;CHENG Yue;JIANG Wei;GAO Yan-rong;TANG Wen-qiang(School of Pharmacy,Shaanxi Institute of International Trade Commerce,Xi’an 712046,China;Co-Innovation Center of Shaanxi Green Manufacturing Technology of Traditional Chianese Medicine,Xi’an 712046,China)
出处
《精细与专用化学品》
CAS
2021年第6期44-47,共4页
Fine and Specialty Chemicals
基金
2020年国家级大学生创新创业训练计划项目(S202013123001)
2020年陕西国际商贸学院校级课题(SMXY202021)。
关键词
苯胺衍生物
吡咯烷侧链
合成
aniline derivative
pyrrolidine side chain
synthesis
