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CAS号114-49-8 氢溴酸东莨菪碱 | CAS号6820-79-7 O-acetylscopolamine | CAS号5027-68-9 [7(S)-(1α,2β,4β...

📜东莨菪碱置于sodium Perchlorate,水体系中,化学反应 3.0H,以83%的收率获得产物去甲东莨菪碱
参考文献:托烷生物碱的电化学n-去甲基化
标题:托烷生物碱的电化学n-去甲基化
摘要:描述了一种实用,有效和选择性的将烷烃生物碱转化为正烷烃衍生物的n-脱甲基方法.降冰片烷,例如去甲肾上腺素和降冰片碱是分别半合成异丙托溴铵或溴托昔铵的重要中间体.合成是使用多孔玻璃碳电极在简单的自制电化学批量电池中进行的.反应在室温下在乙醇或甲醇和水的混合物中一步进行.该方法避免了有害的氧化剂如h 2 ö 2或米氯过苯甲酸(米-Cpba),有毒溶剂(例如氯仿)以及金属基催化剂.在电化学批量或流通池中研究了各种关键参数,并以克级规模在批量和流通池中使用了最佳条件,以方便的液-液萃取方法无需色谱纯化即可以高收率和高纯度合成去甲托品.机理研究表明,电化学的n-去甲基化通过形成亚胺中间体而进行,该亚胺中间体被水转化为亲核试剂.优化后的方法进一步应用于东pol碱,可卡因,苯扎特罗平,荷马特平和托卡卡因,表明这是一种n的通用方法烷对托烷生物碱进行脱甲基,以合成用于医药产品的有价值的前体.
DOI:10.1039/d0Gc00851F

专利信息

专利号:WO-9916526-A1
优先权日:1997-09-30
标题:Method for separating complex mixtures by means of solid phase extraction for use in active substance search and analysis
发明人：GRABLEY SUSANNE; SCHMID INGRID; SATTLER ISABEL; THIERICKE RALF
权利人:HANNS KNOELL INST FUER NATURST; GRABLEY SUSANNE; SCHMID INGRID; SATTLER ISABEL; THIERICKE RALF
摘要:Complex mixtures, such as mixtures of microorganisms, plant or animal assays and synthesis mixtures obtained from combinatory and parallelized synthesis can be separated on the basis of solid phase extraction (SPE). The separation procedure comprises initial adsorption of the complex mixture in suitable separation phases and elution in one or several separation steps each having one or more separation levels. The fractions thus obtained can be concentrated if necessary by means of an additional SPE step or calibrated with a desired solvent. The method is carried out under conditions of gravity, negative pressure or pressures that are substantially lower than those used in high-pressure chromatography.