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盐酸4-甲氧基甲基苯丙胺及其前体的合成与有机杂质剖析

Synthesis and organic impurity profiling of 4-methoxymethamphetamine hydrochloride and its precursors.

作者信息

Tam Rebecca, Heather Erin, Shimmon Ronald, Lam Brandon, McDonagh Andrew M

机构信息

Centre for Forensic Science, University of Technology Sydney, Sydney, NSW 2007, Australia.

Centre for Forensic Science, University of Technology Sydney, Sydney, NSW 2007, Australia.

出版信息

Forensic Sci Int. 2017 Mar;272:184-189. doi: 10.1016/j.forsciint.2016.11.041. Epub 2016 Dec 2.

DOI:10.1016/j.forsciint.2016.11.041
PMID:28065556
Abstract

4-Methoxymethamphetamine (PMMA) was synthesised from star anise and from 4-methoxytoluene and the organic impurity profiles examined. These two starting materials are unrestricted chemicals in many jurisdictions and contain the requisite functional groups and are thus well suited for clandestine manufacturers. trans-Anethole was extracted from star anise and oxidised to 4-methoxyphenyl-2-propanone (PMP2P). 4-Methoxytoluene was oxidised to anisaldehyde, converted to 4-methoxyphenyl-2-nitropropene, and then reduced to PMP2P. The PMP2P obtained by both methods was then converted to PMMA via the Leuckart reaction. 4-Methoxymethamphetamine hydrochloride (PMMA·HCl) was synthesised from PMMA using hydrogen chloride gas. Both of the examined synthetic methods were found to be feasible routes into PMMA·HCl. The products of each step were analysed by gas chromatography-mass spectrometry (GC-MS) and proton nuclear magnetic resonance spectroscopy (H NMR). Impurities were examined in an attempt to identify route specific compounds, which may provide valuable information about the synthetic pathway and precursors.

摘要

4-甲氧基甲基苯丙胺(PMMA)由八角茴香和4-甲氧基甲苯合成,并对有机杂质谱进行了检测。这两种起始原料在许多司法管辖区属于不受管制的化学品,且含有必要的官能团,因此非常适合 clandestine制造商。反式茴香脑从八角茴香中提取并氧化为4-甲氧基苯基-2-丙酮(PMP2P)。4-甲氧基甲苯氧化为茴香醛,转化为4-甲氧基苯基-2-硝基丙烯,然后还原为PMP2P。通过这两种方法得到的PMP2P随后通过吕卡特反应转化为PMMA。4-甲氧基甲基苯丙胺盐酸盐(PMMA·HCl)由PMMA使用氯化氢气体合成。发现所检测的两种合成方法都是合成PMMA·HCl的可行途径。通过气相色谱-质谱联用(GC-MS)和质子核磁共振光谱(H NMR)对每一步产物进行分析。对杂质进行检测,试图识别特定路线的化合物,这可能为合成途径和前体提供有价值的信息。

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