Clandestine manufacture of 3,4-methylenedioxymethylamphetamine (MDMA) by low pressure reductive amination. A mass spectrometric study of some reaction mixtures

Verweij, Anthonie M.A.

doi:10.1016/0379-0738(90)90225-n

Cited by 25 publications

(16 citation statements)

References 2 publications

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“…4 presents other interesting impurities; 3,4-methylenedioxy-N-methylbenzylamine and N,N-dimethyl-MDA, compounds no.°7 and no.°17. These impurities have also been reported as being linked with the reductive amination process [29,36]. Their presence is a good way of noting the differences that can occur between the different possible pathways for this reaction (see Fig.…”

Section: Precursorsmentioning

confidence: 96%

“…These methods are generally simple techniques and require little knowledge of chemistry. Six synthetic pathways using this precursor have been reported [27,28,29,35,36] as being used for making illicit MDMA. These syntheses, described in Figs.…”

Section: Impurity Profilesmentioning

confidence: 99%

“…For MDMA, some workers have reported impurities or by-products [23,24,25,26,27,28,29,30,31], and techniques like Raman spectroscopy [32] or isotope ratio mass spectrometry [33] have been used to link seized tablets.…”

Section: Introductionmentioning

confidence: 99%

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Impurity profiling of seized MDMA tablets by capillary gas chromatography

Palhol¹,

Boyer²,

Naulet³

et al. 2002

Anal Bioanal Chem

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Impurity profiles of 3,4-methylenedioxymethylamphetamine (MDMA) tablets seized in France have been examined. The samples were extracted with methylene chloride under basic conditions and then analyzed by capillary gas chromatography. Almost 30 compounds were identified as precursors, intermediates and by-products. Palmitic and stearic acid were also found as tableting materials. The comparison of the different profiles obtained by the reported procedure provided very useful information about the synthetic processes used by clandestine laboratories and enabled a classification into several groups of profiles. According to these results, the reductive amination route appears to be the most common synthetic pathway in Western Europe. Furthermore, 3,4-methylenedioxyphenyl-2-propanone seems to be the most used precursor in clandestine laboratories.

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Section: Precursorsmentioning

confidence: 96%

Section: Impurity Profilesmentioning

confidence: 99%

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Impurity profiling of seized MDMA tablets by capillary gas chromatography

Palhol¹,

Boyer²,

Naulet³

et al. 2002

Anal Bioanal Chem

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“…Profiling has been done in the past on a variety of drugs including heroin, cocaine, methamphetamine and, most recently, MDMA [14,15,16,17,18]. This process provides a tool that may allow forensic scientists to relate different street drug seizures to a common source based on differences in isolated chemicals.…”

Section: Mdma Detectionmentioning

confidence: 98%

Laboratory and field experiments used to identify Canis lupus var. familiaris active odor signature chemicals from drugs, explosives, and humans

Lorenzo

Wan

Harper

et al. 2003

Analytical and Bioanalytical Chemistry

201

180

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This paper describes the use of headspace solid-phase microextraction (SPME) combined with gas chromatography to identify the signature odors that law enforcement-certified detector dogs alert to when searching for drugs, explosives, and humans. Background information is provided on the many types of detector dog available and specific samples highlighted in this paper are the drugs cocaine and 3,4-methylenedioxy- N-methylamphetamine (MDMA or Ecstasy), the explosives TNT and C4, and human remains. Studies include the analysis and identification of the headspace "fingerprint" of a variety of samples, followed by completion of double-blind dog trials of the individual components in an attempt to isolate and understand the target compounds that dogs alert to. SPME-GC/MS has been demonstrated to have a unique capability for the extraction of volatiles from the headspace of forensic specimens including drugs and explosives and shows great potential to aid in the investigation and understanding of the complicated process of canine odor detection. Major variables evaluated for the headspace SPME included fiber chemistry and a variety of sampling times ranging from several hours to several seconds and the resultant effect on ratios of isolated volatile components. For the drug odor studies, the CW/DVB and PDMS SPME fibers proved to be the optimal fiber types. For explosives, the results demonstrated that the best fibers in field and laboratory applications were PDMS and CW/DVB, respectively. Gas chromatography with electron capture detector (GC/ECD) and mass spectrometry (GC/MS) was better for analysis of nitromethane and TNT odors, and C-4 odors, respectively. Field studies with detector dogs have demonstrated possible candidates for new pseudo scents as well as the potential use of controlled permeation devices as non-hazardous training aids providing consistent permeation of target odors.

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“…More authors prefer to focus on the identification of impurities in freshly prepared MDMA samples via different synthesis routes and give us analytical data of precursors, intermediates and reaction by products [8][9][10][11][12][13][14][15][16][17][18]. Among published extraction processes, one consists in dissolving 5 mg of crushed MDMA tablets into 1 ml of redistilled diethyl ether [4].…”

Section: Introductionmentioning

confidence: 99%

Optimization of extraction parameters for the chemical profiling of 3,4-methylenedioxymethamphetamine (MDMA) tablets

Gimeno

Besacier

Chaudron-Thozet

2003

Forensic Science International

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The extraction of impurities from illegally produced 3,4-methylenedioxymethamphetamine (MDMA) has been studied in order to optimize the parameters. Two different MDMA samples were used. Particular attention was paid to the influence of the pH, the evaporation step, and the sample storage. The method used was an extraction of impurities by diethyl ether from a buffer solution at pH 11.5, followed by gas chromatography (GC) mass spectrometric (MS) analyses after a dryness concentration under monitored conditions of the ethereal extract. Repeat extractions of the same sample gave an average relative standard deviation (RSD) of less than 8.5% within day and less than 10.5% between days. #

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Clandestine manufacture of 3,4-methylenedioxymethylamphetamine (MDMA) by low pressure reductive amination. A mass spectrometric study of some reaction mixtures

Cited by 25 publications

References 2 publications

Impurity profiling of seized MDMA tablets by capillary gas chromatography

Impurity profiling of seized MDMA tablets by capillary gas chromatography

Laboratory and field experiments used to identify Canis lupus var. familiaris active odor signature chemicals from drugs, explosives, and humans

Optimization of extraction parameters for the chemical profiling of 3,4-methylenedioxymethamphetamine (MDMA) tablets

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