一种坎地沙坦酯中间体的合成方法

文档序号:143913 发布日期:2021-10-22 浏览:24次 >En<

阅读说明:本技术 一种坎地沙坦酯中间体的合成方法 (Synthesis method of candesartan cilexetil intermediate ) 是由 涂国良 黄健升 张露 杨涛 梁尊俊 于 2019-01-02 设计创作,主要内容包括:一种式(II)所示的坎地沙坦酯中间体的合成方法,其包括:(1)将式(IV)所示的化合物溶解于非质子溶剂中,得到第一混合液;将相转移催化剂及叠氮化试剂溶解于水中,得到第二混合液;(2)将第一混合液滴加至第二混合液中进行叠氮化反应,反应结束后,静置分层,得到含有式(V)所示化合物的有机相;(3)将所得到的含有式(V)所示化合物的有机相滴加到叔丁醇中进行重排反应,反应结束后,浓缩得到固体或油状物,然后向所得固体或油状物中加入结晶溶剂重结晶,分离得到晶体,即式(II)所示的坎地沙坦酯中间体。本申请的合成方法不需使用DMF溶剂,安全环保,减少氨氮废水产生。(A method for synthesizing candesartan cilexetil intermediate shown in formula (II) comprises the following steps: (1) dissolving a compound shown as a formula (IV) in an aprotic solvent to obtain a first mixed solution; dissolving a phase transfer catalyst and an azide reagent in water to obtain a second mixed solution; (2) dropwise adding the first mixed solution into the second mixed solution to carry out an azide reaction, and after the reaction is finished, standing and layering to obtain an organic phase containing the compound shown in the formula (V); (3) dropwise adding the obtained organic phase containing the compound shown in the formula (V) into tert-butanol for rearrangement reaction, concentrating to obtain a solid or oily substance after the reaction is finished, adding a crystallization solvent into the obtained solid or oily substance for recrystallization, and separating to obtain crystals, namely the candesartan cilexetil intermediate shown in the formula (II). The synthetic method does not need a DMF solvent, is safe and environment-friendly, and reduces the generation of ammonia nitrogen wastewater.)

18页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:通过还原胺化制备多亚烷基多胺

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!