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由α-苯乙酰乙腈(APAAN)合成的甲基苯丙胺的杂质剖析

Impurity profiling of methamphetamine synthesised from α-phenylacetoacetonitrile (APAAN).

作者信息

Langone Deanna, Painter Ben, Nash Clark, Johnston Martin R, Kirkbride K Paul

机构信息

College of Science and Engineering, Flinders University, Adelaide, South Australia, Australia.

Forensic Science SA, Adelaide, South Australia, Australia.

出版信息

Drug Test Anal. 2022 Jan;14(1):56-71. doi: 10.1002/dta.3140. Epub 2021 Aug 18.

DOI:10.1002/dta.3140
PMID:34355528
Abstract

The rise in popularity of 'designer' precursor compounds for the synthesis of amphetamine-type stimulants poses a significant challenge to law enforcement agencies. One such precursor is α-phenylacetoacetonitrile (APAAN). APAAN emerged in Europe in 2010 and quickly became one of the most popular precursors for amphetamine synthesis in that region. Previous literature has identified four APAAN-specific impurities formed in the synthesis of amphetamine; however, there is currently no research on the use of APAAN in the synthesis of methamphetamine, which is more likely to be employed in a non-European market. In this study methamphetamine was synthesised via three common clandestine methods: the Leuckart method and two reductive amination methods. We report the identification of five new impurities and two previously identified impurities characteristic for the use of APAAN in the synthesis of methamphetamine. The newly identified impurities were characterised by MS and NMR and determined to be (E)-3-(methylamino)-2-phenylbut-2-enenitrile, 3-(methylamino)-2-phenylbutanenitrile, 3-methyl-2,4-diphenylpentanedinitrile, 2-phenylbutyronitrile and 3-hydroxy-2-phenylbutanenitrile.

摘要

用于合成苯丙胺类兴奋剂的“设计型”前体化合物日益流行,这给执法机构带来了重大挑战。其中一种前体是α-苯基乙酰乙腈(APAAN)。APAAN于2010年在欧洲出现,并迅速成为该地区合成苯丙胺最常用的前体之一。以往文献已鉴定出在合成苯丙胺过程中形成的四种特定于APAAN的杂质;然而,目前尚无关于APAAN用于合成甲基苯丙胺的研究,而甲基苯丙胺更可能在非欧洲市场使用。在本研究中,通过三种常见的秘密方法合成了甲基苯丙胺:勒卡特法和两种还原胺化法。我们报告了鉴定出的五种新杂质以及两种先前鉴定出的、特定于APAAN用于合成甲基苯丙胺的杂质。新鉴定出的杂质通过质谱和核磁共振进行了表征,确定为(E)-3-(甲氨基)-2-苯基丁-2-烯腈、3-(甲氨基)-2-苯基丁腈、3-甲基-2,4-二苯基戊二腈、2-苯基丁腈和3-羟基-2-苯基丁腈。

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