Isotope fractionation during the synthesis of MDMA.HCl from helional

Cormick, Justin; Carter, James F.; Currie, Timothy; Matheson, Carney; Cresswell, Sarah L.

doi:10.1016/j.forc.2022.100406

Cited by 3 publications

(13 citation statements)

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“…However, this nitrogen atom is lost when MDP2P is prepared from MDP2NP, and a new nitrogen source is then required when MDMA is synthesised from MDP2P. Previous research [3][4][5][6][7] has shown some δ 15…”

Section: Resultsmentioning

confidence: 99%

“…Collins et al 12 Piperonal to MDP2NP: To N-butylamine (0.249 g) in 10 mL of ethanol were added piperonal (10.0199 g, 0.066741 mol) and nitroethane (5.357 g) under N 2 . The reaction was heated at reflux for 24 h. After cooling the resulting precipitate was collected with vacuum filtration, washed with cold ethanol and dried in a vacuum desiccator over phosphorus pentoxide to give yellow crystals during the synthesis of MDMA from MDP2P [4][5][6][7] and during the HCl salt precipitation of MDA and MDMA. 7 An interesting pattern emerged in δ 2 H composition when the results presented here were compared to those of Collins et al 12 for the synthesis of amphetamine from benzaldehyde (Figure 3).…”

Section: Synthesismentioning

confidence: 99%

“…The reaction was heated at reflux for 24 h. After cooling the resulting precipitate was collected with vacuum filtration, washed with cold ethanol and dried in a vacuum desiccator over phosphorus pentoxide to give yellow crystals during the synthesis of MDMA from MDP2P [4][5][6][7] and during the HCl salt precipitation of MDA and MDMA. 7 An interesting pattern emerged in δ 2 H composition when the results presented here were compared to those of Collins et al 12 for the synthesis of amphetamine from benzaldehyde (Figure 3). Essentially, the more positive the δ 2 H value of the precursor the greater the negative shift in δ 2 H value during the preparation of P2NP and MDP2NP, through to amphetamine, MDP2P and MDA.…”

Section: Synthesismentioning

confidence: 99%

“…Previous research into the IRMS analysis of MDA/MDMA suggests minimal information can be obtained about the synthetic history of samples. [3][4][5][6][7] IRMS data have, however, been used to compare batch-to-batch variations and provide information for law enforcement.…”

Section: Introductionmentioning

confidence: 99%

“…Isotope ratio mass spectrometry (IRMS) has been used as an additional method of analysis that can provide important information for illicit drug profiling, particularly when used in combination with other techniques (such as impurity profiling). Previous research into the IRMS analysis of MDA/MDMA suggests minimal information can be obtained about the synthetic history of samples 3–7 . IRMS data have, however, been used to compare batch‐to‐batch variations and provide information for law enforcement.…”

Section: Introductionmentioning

confidence: 99%

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Stable isotope characterisation of 3,4‐methylenedioxyphenyl‐2‐propanone and 3,4‐methylenedioxyamphetamine prepared from piperonal

Cormick

Carter

Currie

et al. 2022

Rapid Comm Mass Spectrometry

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Rationale Stable isotopic ratios can provide information for illicit drug profiling. The research presented here investigated the variations in stable isotopic ratios of hydrogen (δ2H), carbon (δ13C), nitrogen (δ15N) and oxygen (δ18O) during the synthesis of MDP2P (3,4‐methylenedioxyphenyl‐2‐propanone) and MDA (3,4‐methylenedioxyamphetamine) prepared via the ‘nitrostyrene’ route. Methods Samples of MDA and MDP2P were synthesised from two isotopically characterised starting materials, piperonal and nitroethane. The isotopic compositions of the nitrostyrene intermediate (3,4‐methylenedioxyphenyl‐2‐nitropropene, MDP2NP) and products MDP2P and MDA were also measured by isotope ratio mass spectrometry. Results A significantly negative change occurred to δ2H values during the production of MDP2NP, MDP2P and MDA, indicating a mechanism that favours inclusion or retention of 1H over 2H. This suggests that the δ2H compositions of MDA/MDP2P prepared from piperonal will not provide information on the synthetic history. Minimal changes were observed in δ13C composition during the synthesis of MDP2NP, MDP2P and MDA, and minimal δ15N compositional changes occurred in MDP2NP and MDA. Progressing from piperonal to MDP2NP, a minimal change occurred to δ18O composition. A variable change to δ18O was observed from MDP2NP with one sample becoming more positive in δ18O composition and two samples becoming more negative. Progressing from MDP2NP to MDA, a significant negative change occurred to δ18O composition. Conclusions The changes to stable isotopic ratios observed during the preparation of MDA and MDP2P from piperonal may prove useful when attempting to compare batch‐to‐batch variations between seizures and provide information with tactical intelligence applications.

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Section: Resultsmentioning

confidence: 99%

Section: Synthesismentioning

confidence: 99%

Section: Synthesismentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Stable isotope characterisation of 3,4‐methylenedioxyphenyl‐2‐propanone and 3,4‐methylenedioxyamphetamine prepared from piperonal

Cormick

Carter

Currie

et al. 2022

Rapid Comm Mass Spectrometry

Self Cite

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The synthesis of MDA from helional and characterisation by isotope ratio mass spectrometry

Cormick

Carter²,

Currie³

et al. 2022

Forensic Chemistry

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Intelligence and the Value of Forensic Science

Speaker

2024

Forensic Sciences

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Recent research has seen a rapid expansion in the reference to front-end forensics as an indication of the untapped value of forensic science. While some of these contributions have centered on development of forensic intelligence from a single area of investigation, others call for a more fundamental change in the relationship between crime laboratories and policing, particularly relating early laboratory analysis with big datasets to provide leads to investigators. We highlight several recently implemented tactical strategies of crime laboratories that contribute to the body of forensic intelligence. Beyond the scientific gains from these tactical applications, the corresponding details on associated efficiencies, costs, time savings, and quality improvements offer insights towards patterns of success for the community of crime laboratories. Further details expand an interpretation of what constitutes success with an eye on the contributions of the crime laboratory towards public health, safety, and protection of the innocent in addition to societal gains from conviction of the guilty. The economic interpretation of the value provided by the forensic laboratory assists in the cost–benefit review of strategic and tactical decisions and supports the justification for laboratory public funding with measures of the return on investment from public support of the forensic laboratory. Examples of the cost savings from crimes avoided include the returns from testing the backlog of unsubmitted sexual assault kits with USD 81 of costs avoided for each USD 1 spent to high-efficiency laboratories achieving gains of USD 646 for each UD 1 spent on de novo case submissions.

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Isotope fractionation during the synthesis of MDMA.HCl from helional

Cited by 3 publications

References 28 publications

Stable isotope characterisation of 3,4‐methylenedioxyphenyl‐2‐propanone and 3,4‐methylenedioxyamphetamine prepared from piperonal

Stable isotope characterisation of 3,4‐methylenedioxyphenyl‐2‐propanone and 3,4‐methylenedioxyamphetamine prepared from piperonal

The synthesis of MDA from helional and characterisation by isotope ratio mass spectrometry

Intelligence and the Value of Forensic Science

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