Step 2: Reaction with POCl3 The reaction mixture from step 1 is added...

August 22, 2024 at 3:29 PM  ·  Comment — Archer T. Ships replied to his own comment.  ·  View on Facebook  ·  Markdown source

Step 2: Reaction with POCl3 The reaction mixture from step 1 is added slowly to a solution of phosphorus oxychloride (POCl3, 150 g, 0.9 mol) in dichloromethane (500 mL) under ice cooling. The resulting mixture is stirred for 30 minutes and then heated at reflux for 2 hours. Step 3: Purification The reaction mixture is cooled to room temperature, poured into a separatory funnel containing cold water (500 mL), and extracted with dichloromethane (3 x 200 mL). The combined organic layers are washed with brine, dried over MgSO4, and concentrated under reduced pressure using a rotary evaporator. The crude product is purified by recrystallization from hexane to yield pure MPP. Step 4: Reduction of MPP MPP (50 g, 0.2 mol) is added to a solution of lithium aluminum hydride (LiAlH4, 30 g, 0.8 mol) in tetrahydrofuran (THF, 500 mL). The mixture is refluxed for 3 hours, cooled to room temperature, and then carefully hydrolyzed with water. The resulting solid is filtered off, and the filtrate is concentrated under reduced pressure. Step 5: Purification of 3-MeO-PCP The crude product from step 4 is purified by column chromatography using silica gel as the stationary phase and a mixture of dichloromethane and methanol as the mobile phase. The desired compound, 3-MeO-PCP, elutes as a yellow oil. Quality Testing: Melting point determination: Determine the melting point range of the purified product using a capillary tube in a melting point apparatus. NMR spectroscopy: Obtain proton (1H) and carbon (13C) NMR spectra of the purified product to confirm its structure and purity. Mass spectrometry: Obtain an electrospray ionization mass spectrum (ESI-MS) or matrix-assisted laser desorption/ionization time-of-flight mass spectrum (MALDI-TOF MS) to confirm the molecular weight and formula of the compound. Elemental analysis: Determine the elemental composition of the purified product using techniques such as X-ray fluorescence (XRF) or inductively coupled plasma atomic emission spectroscopy (ICP-AES). Note: This synthetic pathway is for research purposes only and not intended for illicit drug synthesis or distribution. It is essential to follow proper safety protocols, dispose of waste materials responsibly, and adhere to local and international laws governing the possession and manufacture of controlled substances. ¹From the Street to the Laboratory: Analytical Profiles of Methoxetamine, 3-Methoxyeticyclidine and 3-Methoxyphencyclidine and their Determination in Three Biological Matrices | Journal of Analytical Toxicology | Oxford Academic ²From the Street to the Laboratory: Analytical Profiles of Methoxetamine, 3-Methoxyeticyclidine and 3-Methoxyphencyclidine and their Determination in Three Biological Matrices | Journal of Analytical Toxicology | Oxford Academic