阿尼利定和匹米诺定的新合成方法研究
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- 英文论文题名：A convenient preparation of anileridine and piminodine
- 论文作者：高振华 ; 郭永彪 ; 孟祥燕 ; 何小伟 ; 邹传品
- 英文论文作者：Zhenhua Gao ; Yongbiao Guo ; Xiangyan Meng ; Xiaowei He ; Chuanpin Zou ; Research Institute of Chemical Defense
- 年：2016
- 作者机构：防化研究院;
- 论文关键词：阿尼利定 ; 匹米诺定 ; 哌啶 ; 合成
- 英文论文关键词：anileridine ; piminodine ; piperidine ; synthesis
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第三十四分会：公共安全化学
- 语种：中文
- 分类号：TQ460.6
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第三十四分会 ; 公共安全化学
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：163k
- 原文格式：D
- 会议级别：全国
摘要
本文首先以苯乙腈为原料经一锅法合成磺酸酯1,然后磺酸酯1分别与二胺6和7反应合成哌啶2和4,最后哌啶2和4在酸性条件下发生醇解反应完成对阿尼利定(anileridine)和匹米诺定(piminodine)的合成。在对哌啶2和4的合成中主要考察了二胺的用量,反应温度和反应时间对反应产率造成的影响,得到的最佳反应条件为:二胺6和7的用量为3~4 eq,反应温度120?C,反应时间18 h。通过反应条件筛选,提高了磺酸酯1和二胺6、7环合反应的选择性,得到了很好的产率。与传统方法相比,本文所采用的方法反应路线短、效率高。
An efficient method for the preparation of anileridine and piminodine has been developed: the bis-mesylate 1 was synthesized by one-pot reaction, then the key piperidine intermediate 2(4) was synthesized via the cyclization of bis-mesylate 1 with diamine 6(7), finally anileridine(piminodine) was obtained easily from piperidine 2(4) by alcoholysis reaction using Et OH/H_2SO_4. Various cyclization conditions of bis-mesylate 1 with diamine 6(7) were examined, and the optimum reaction condition was established: diamine 3~4 eq, reaction temperature 120°C, reaction time18 h.
An efficient method for the preparation of anileridine and piminodine has been developed: the bis-mesylate 1 was synthesized by one-pot reaction, then the key piperidine intermediate 2(4) was synthesized via the cyclization of bis-mesylate 1 with diamine 6(7), finally anileridine(piminodine) was obtained easily from piperidine 2(4) by alcoholysis reaction using Et OH/H_2SO_4. Various cyclization conditions of bis-mesylate 1 with diamine 6(7) were examined, and the optimum reaction condition was established: diamine 3~4 eq, reaction temperature 120°C, reaction time18 h.
引文
[1]Asano,S.;Ban,H.Heterocycles,2008,75,183.
[2]高振华,何小伟,郭永彪,邹传品.波谱学杂志.2014,31,284.
[2]高振华,何小伟,郭永彪,邹传品.波谱学杂志.2014,31,284.