10.1002/chir.20957
The study aims to develop a chiral gas chromatographic method for separating compounds involved in the EMDE synthesis of methylamphetamine, a widely abused stimulant drug. The chemicals involved include ephedrine, pseudoephedrine, chlorinated intermediates, and methylamphetamine, which are the primary compounds of interest in the synthesis process. The researchers used fluorinated acid anhydrides such as trifluoroacetic anhydride (TFAA), pentafluoropropanoic anhydride (PFPA), and heptafluorobutyric anhydride (HFBA) as chemical derivatization reagents to reduce the polarity and basicity of these compounds, thereby improving enantiomeric separations. The study focused on separating the enantiomers of these compounds using a 2,3-di-O-methyl-6-t-butyl silyl-b-cyclodextrin stationary phase (CHIRALDEXTM B-DM) in a gas chromatograph. The results showed that PFPA derivatization effectively separated the enantiomers of pseudoephedrine, methylamphetamine, and chlorinated intermediates within 40 minutes, while TFAA was used for ephedrine enantiomers. The study concludes that this method can help identify the source of starting materials and synthetic routes used in the illicit manufacture of methylamphetamine, particularly distinguishing the Emde route from other methods like Birch reduction and Nagai methods.
10.1021/jacs.9b08176
The study focuses on the synthesis and characterization of disodium salts of pseudoephedrine-derived Myers enolates, which are used in alkylation reactions to produce chiral compounds with high yields and stereoselectivities. The chemicals used include sodium diisopropylamide (NaDA) as the base to generate the enolates, various alkyl halides for alkylation, and tetrahydrofuran (THF) as the solvent. The purpose of these chemicals is to investigate the reactivity and selectivity of the disodium enolates in comparison to the dilithium salts, with the aim of developing a more efficient and industrially viable protocol for alkylation reactions. The study also explores the structural and mechanistic aspects of these enolates, using techniques such as NMR spectroscopy, IR spectroscopy, and density functional theory (DFT) computations to understand their aggregation states and reaction mechanisms.