Investigation of the reaction impurities associated with methylamphetamine synthesized using the nagai method

Vanitha Kunalan, Niamh Nic Daeid, William Kerr

Research output: Contribution to journalArticle

16 Citations (Scopus)

Abstract

The synthesis of methylamphetamine hydrochloride from l-ephedrine or d-pseudoephedrine hydrochloride via reduction with hydriodic acid and red phosphorus was investigated. Eighteen batches of methylamphetamine hydrochloride were synthesized in six replicate batches using three different reaction times. This allowed the investigation of the variation of impurities in the final product with reaction time. The results obtained have resolved previously conflicting impurity profile data reported in the literature for this synthesis route. The impurity profile was shown to change with reaction time and all previously. reported impurity components were identified but not in all batches. Additionally, 20 batches of methylamphetamine hydrochloride were synthesized from either from l-ephedrine or d-pseudoephedrine hydrochloride in reactions which were allowed to proceed for 24 h. The impurities present in the resulting batches were investigated, and route-specific impurities present in all batches were identified. Batch-to-batch fluctuations in the resultant chromatographic impurity profile, despite careful synthetic monitoring and control, were also noted.

LanguageEnglish
Pages5744-5752
Number of pages9
JournalAnalytical Chemistry
Volume84
Issue number13
DOIs
Publication statusPublished - 31 May 2012

Fingerprint

Methamphetamine
Impurities
Pseudoephedrine
Ephedrine
lissamine rhodamine B
Phosphorus
Monitoring

Keywords

  • methylamphetamine hydrochloride
  • impurity profile
  • impurity components

Cite this

@article{e129b6fb28e140c6a69a9c85471143fe,
title = "Investigation of the reaction impurities associated with methylamphetamine synthesized using the nagai method",
abstract = "The synthesis of methylamphetamine hydrochloride from l-ephedrine or d-pseudoephedrine hydrochloride via reduction with hydriodic acid and red phosphorus was investigated. Eighteen batches of methylamphetamine hydrochloride were synthesized in six replicate batches using three different reaction times. This allowed the investigation of the variation of impurities in the final product with reaction time. The results obtained have resolved previously conflicting impurity profile data reported in the literature for this synthesis route. The impurity profile was shown to change with reaction time and all previously. reported impurity components were identified but not in all batches. Additionally, 20 batches of methylamphetamine hydrochloride were synthesized from either from l-ephedrine or d-pseudoephedrine hydrochloride in reactions which were allowed to proceed for 24 h. The impurities present in the resulting batches were investigated, and route-specific impurities present in all batches were identified. Batch-to-batch fluctuations in the resultant chromatographic impurity profile, despite careful synthetic monitoring and control, were also noted.",
keywords = "methylamphetamine hydrochloride , impurity profile , impurity components",
author = "Vanitha Kunalan and Daeid, {Niamh Nic} and William Kerr",
year = "2012",
month = "5",
day = "31",
doi = "10.1021/ac3009302",
language = "English",
volume = "84",
pages = "5744--5752",
journal = "Analytical Chemistry",
issn = "0003-2700",
publisher = "American Chemical Society",
number = "13",

}

Investigation of the reaction impurities associated with methylamphetamine synthesized using the nagai method. / Kunalan, Vanitha; Daeid, Niamh Nic; Kerr, William.

In: Analytical Chemistry, Vol. 84, No. 13, 31.05.2012, p. 5744-5752.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Investigation of the reaction impurities associated with methylamphetamine synthesized using the nagai method

AU - Kunalan, Vanitha

AU - Daeid, Niamh Nic

AU - Kerr, William

PY - 2012/5/31

Y1 - 2012/5/31

N2 - The synthesis of methylamphetamine hydrochloride from l-ephedrine or d-pseudoephedrine hydrochloride via reduction with hydriodic acid and red phosphorus was investigated. Eighteen batches of methylamphetamine hydrochloride were synthesized in six replicate batches using three different reaction times. This allowed the investigation of the variation of impurities in the final product with reaction time. The results obtained have resolved previously conflicting impurity profile data reported in the literature for this synthesis route. The impurity profile was shown to change with reaction time and all previously. reported impurity components were identified but not in all batches. Additionally, 20 batches of methylamphetamine hydrochloride were synthesized from either from l-ephedrine or d-pseudoephedrine hydrochloride in reactions which were allowed to proceed for 24 h. The impurities present in the resulting batches were investigated, and route-specific impurities present in all batches were identified. Batch-to-batch fluctuations in the resultant chromatographic impurity profile, despite careful synthetic monitoring and control, were also noted.

AB - The synthesis of methylamphetamine hydrochloride from l-ephedrine or d-pseudoephedrine hydrochloride via reduction with hydriodic acid and red phosphorus was investigated. Eighteen batches of methylamphetamine hydrochloride were synthesized in six replicate batches using three different reaction times. This allowed the investigation of the variation of impurities in the final product with reaction time. The results obtained have resolved previously conflicting impurity profile data reported in the literature for this synthesis route. The impurity profile was shown to change with reaction time and all previously. reported impurity components were identified but not in all batches. Additionally, 20 batches of methylamphetamine hydrochloride were synthesized from either from l-ephedrine or d-pseudoephedrine hydrochloride in reactions which were allowed to proceed for 24 h. The impurities present in the resulting batches were investigated, and route-specific impurities present in all batches were identified. Batch-to-batch fluctuations in the resultant chromatographic impurity profile, despite careful synthetic monitoring and control, were also noted.

KW - methylamphetamine hydrochloride

KW - impurity profile

KW - impurity components

UR - http://www.scopus.com/inward/record.url?scp=84863477448&partnerID=8YFLogxK

U2 - 10.1021/ac3009302

DO - 10.1021/ac3009302

M3 - Article

VL - 84

SP - 5744

EP - 5752

JO - Analytical Chemistry

T2 - Analytical Chemistry

JF - Analytical Chemistry

SN - 0003-2700

IS - 13

ER -