The Significance of 99% Purity PMK Ethyl Glycidate in Chemical Synthesis
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PMK ethyl glycidate, a compound of considerable importance in organic chemistry, serves as a pivotal intermediate in the synthesis of various complex molecules, particularly in the production of certain illicit substances. Understanding its properties, production, and applications is crucial for chemists and pharmaceutical manufacturers. The emphasis on achieving 99% purity in PMK ethyl glycidate is not merely a benchmark; it is a vital standard that underpins the quality and effectiveness of the final products.
Chemical Structure and Characteristics
PMK ethyl glycidate, chemically known as (2S,3S)-3-ethoxy-2-methyl-1,3-oxolan-2-yl acetate, belongs to the class of glycidate esters. This compound features an epoxide group, which is primarily responsible for its reactivity in various synthetic pathways. The purity of such a compound is paramount&#;99% purity indicates that there is minimal contamination from isomers or byproducts, which could adversely affect chemical reactions or lead to unwanted side effects in drug formulations.
Synthesis and Purification
The synthesis of PMK ethyl glycidate involves several chemical reactions starting from simpler organic materials. Typically, precursors like phenyl-2-propanone (P2P) are transformed through a series of steps, including esterification and subsequent cyclization. Achieving high purity levels in the final product often necessitates advanced purification techniques, such as distillation, recrystallization, or chromatography. These methods not only improve the yield but also ensure that the compound meets the strict standards required for industrial applications.
Industrial Applications
In the pharmaceutical industry, 99% purity PMK ethyl glycidate is particularly valuable for its role in synthesizing various pharmaceutical agents. Its utility extends beyond simple applications; it is a critical intermediate in producing modified molecules that exhibit specific biological activities. This is particularly relevant in the development of novel therapies and drug formulations, where the efficacy and safety of the product are paramount.
Moreover, PMK ethyl glycidate is often a precursor in the synthesis of controlled substances. While this underscores its value in certain research contexts, it also highlights the need for stringent regulatory measures to prevent misuse. The synthesis and handling of this compound must be conducted within the legal frameworks established by government bodies to ensure ethical standards in research and manufacturing.
Quality Control and Regulatory Compliance
Due to the significance of PMK ethyl glycidate in both legitimate and illicit contexts, maintaining high purity levels is integral to quality control processes in the manufacturing environment. Regulatory agencies such as the FDA and EMA maintain strict guidelines regarding the quality of chemical compounds used in pharmaceutical production. Continual monitoring for contaminants and adherence to Good Manufacturing Practices (GMP) are essential for firms engaged in the synthesis of this compound.
Conclusion
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In summary, the importance of 99% purity PMK ethyl glycidate in chemical synthesis cannot be overstated. Not only does it serve as a critical building block for various organic compounds, but it is also essential for ensuring the efficacy and safety of pharmaceutical products. As the demand for high-quality intermediates continues to grow, an appreciation for the intricacies of synthesizing and purifying compounds like PMK ethyl glycidate becomes increasingly relevant. Striking a balance between innovation in synthesis and adherence to regulatory standards will be key to advancing pharmaceutical science while minimizing potential risks associated with misuse.
PMK ethyl glycidate can be used as organic synthesis intermediate and pharmaceutical intermediate, mainly used in laboratory research and development process and pharmaceutical chemical production process.
Fig. 1 The synthetic step 1 of PMK ethyl glycidate.
To a solution of piperonal (1, 3.00 g, 19.9 mmol) in CH2Cl2 (100 mL) was added (carbethoxyethylidene)triphenylphosphorane (2,14.5 g, 40.0 mmol), and the reaction mixture was stirred for 24 h at room temperature. The mixture was then concentrated at reduced pressure, and the residue was purified by flash column chromatography on silica gel (hexanes/EtOAc,10:1) to afford olefin 3 (4.45 g, 95%) as a colorless oil: 1H NMR (400 MHz, CDCl3) d 7.58 (s, 1H), 6.92 (d, J = 1.7 Hz, 1H), 6.90 (dd, J = 7.9, 1.7 Hz, 1H), 6.82 (d, J = 8.0 Hz, 1H), 5.97 (s, 2H), 4.24 (q, J = 7.1 Hz, 2H), 2.10 (d, J = 1.6 Hz, 3H),1.33 (t, J = 7.1 Hz, 3H); 13C NMR (100 MHz, CDCl3) d 168.7,147.6, 138.3, 129.9, 126.9, 124.6, 109.5, 108.2, 101.2, 60.7, 14.3,1 4.0; IR (ATR, cm-1): , ,, , , ,, , ; HRMS (EI) m/z calcd for C13H14O4 (M+) 234., found 234. [1].
Fig. 2 The synthetic step 2 of PMK ethyl glycidate.
To a solution of olefin 3 (3.00 g, 12.8 mmol) in CH2Cl2 (80 mL) was added 50&#;55% m-chloroperbenzoic acid (6.2 g,17.9 mmol). The reaction mixture was refluxed for 24 h, cooled to room temperature, quenched with 10% aqueous sodium sulfite (30 mL), and diluted with CH2Cl2 (100 mL). The organic layer was separated, and the aqueous layer was extracted with CH2Cl2 (2 × 30 mL). The combined organic layers were washed with saturated aqueous NaHCO3 and brine, dried over anhydrous MgSO4, and concentrated at reduced pressure. The resulting residue was purified by flash column chromatography on silica gel (hexanes/EtOAc, 10:1) to afford epoxide 4 (2.12 g, 66%) as a colorless oil: 1H NMR (400 MHz, CDCl3) d 6.79 (d, J = 1.6 Hz, 2H), 6.76 (s, 1H), 5.96 (d, J = 1.6 Hz, 2H), 4.30&#;4.17 (m, 2H), 4.21 (s, 1H), 1.31 (ddd, J = 8.8, 8.8, 1.7 Hz, 6H); 13C NMR (100 MHz, CDCl3) d 170.8, 147.7, 147.6, 127.6, 120.3, 108.2, 107.0, 101.2, 62.2, 61.8, 59.9, 14.1, 12.5; IR (ATR, cm-1) , , , , , , , ; HRMS (EI) m/z calcd for C13H14O5 (M+) 250., found 250. [1].
PMK ethyl glycidate as an intermediate in the synthesis of M-ALPHA analog and MDMA. The widespread abuse of illicit psychoactive substances is one of the most serious public health and social problems. A suspicious airmail package was seized by Korean customs, and two psychoactive substances in the grayish-green pills in the package were detected by ultra-performance liq. chromatog. The structures of the two substances were elucidated by a combination of liq. chromatog. quadrupole time-of-flight mass spectrometry, NMR spectroscopy, and comparison with reported or newly generated spectral data of the suggested structures. One of the psychoactive substances proved to be MDMA (commonly known as "Ecstasy"), and the other compd. was an M-ALPHA analog bearing a hydroxyl group and an N-methylcarboxamide group. The new M-ALPHA analog was detd. as 3-(benzo[d][1,3]dioxol-5-yl)-2-hydroxy-N,2-dimethyl-3-(methylamino)propanamide and named as M-ALPHA-HMCA, wherein HMCA denotes hydroxymethylcarboxamide. Although psychoactivity of this compd. has not been assessed, M-ALPHA-HMCA should be considered a potential new psychoactive substance and/or a byproduct of MDMA [1].
PMK ethyl glycidate as an intermediate in the synthesis of desoxy phenethylamine analogs. The desoxy phenethylamine analogs in this study represent a combination of alkyl side-chain and cyclic amines (azetidine, pyrrolidine, piperidine and azepane) to yield a set of mols. of identical elemental compn. as well as major mass spectral fragment ions (base peaks) of identical elemental compn. These desoxy phenethylamine analogs of the aminoketone designer drug, 3,4-methylenedioxy-pyrrovalerone (MDPV) related to the natural product cathinone were prepd. from piperonal (3,4-methylenedioxybenzaldehyde) via the intermediate precursor ketones. The aminoketones and the desoxy phenethylamine regioisomers were each sepd. in capillary gas chromatog. expts. using an Rxi-7Sil MS stationary phase with the aminoketones showing greater retention than the corresponding desoxyamines[2].
[1] Lee J H, Park O R, Mandava S, et al. Identification of a new M-ALPHA analog and MDMA in an illegal health product[J]. Forensic science international, , 313: .
[2] Abiedalla Y, DeRuiter J, Clark C R. GC&#;MS, GC&#;MS/MS and GC-IR differentiation of desoxy cathinone derivatives: cyclic tertiary amines related to MDPV[J]. Journal of Chromatography B, , : 38-48.