- The molecular structure and vibrational, 1H and 13C NMR spectra of lidocaine hydrochloride monohydrate
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The structure, vibrational and NMR spectra of the local anesthetic drug lidocaine hydrochloride monohydrate salt were investigated by B3LYP/6-311G calculations. The lidocaine·HCl·H2O salt is predicted to have the gauche structure as the predominant form at ambient temperature with NCCN and CNCC torsional angles of 110° and -123° as compared to 10° and -64°, respectively in the base lidocaine. The repulsive interaction between the two N-H bonds destabilized the gauche structure of lidocaine·HCl·H2O salt. The analysis of the observed vibrational spectra is consistent with the presence of the lidocaine salt in only one gauche conformation at room temperature. The 1H and 13C NMR spectra of lidocaine·HCl·H2O were interpreted by experimental and DFT calculated chemical shifts of the lidocaine salt. The RMSD between experimental and theoretical 1H and 13C chemical shifts for lidocaine·HCl·H2O is 2.32 and 8.21 ppm, respectively.
- Badawi, Hassan M.,F?rner, Wolfgang,Ali, Shaikh A.
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- Preparation method of lidocaine hydrochloride
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The invention relates to a preparation method of lidocaine hydrochloride, which comprises the following steps: carrying out acylation reaction by using 2, 6-dimethylaniline and chloroacetyl chloride as raw materials, directly adding diethylamine into the system to carry out amination reaction after the reaction is finished, filtering the product, and adding hydrochloric acid into the filtrate to carry out salification reaction. The preparation method of lidocaine hydrochloride provided by the invention is a one-pot method, avoids repeated purification of an intermediate product in a traditional process, and is simple in process, mild in condition, easy to control, high in product yield and high in purity.
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- Method for preparing lidocaine hydrochloride
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The invention provides a method for preparing lidocaine hydrochloride, and belongs to the technical field of anesthetic synthesis. The method comprises the following steps: by taking 2,6-xylenol as a raw material, Pd/C as a main catalyst and 2,6-dimethylcyclohexanone as a promoter, performing liquid phase amination with ammonia water at high temperature, thereby obtaining a midbody 2,6-dimethylaniline; enabling sodium methylate, 2,6-dimethylaniline and N,N-lignocaine methyl acetate as raw materials to react at 90-95 DEGC, distilling while reaction is performed to remove methanol till no methanol can be evaporated out, continuously reacting for 30 minutes, cooling to the room temperature, adding dichloroethane, washing with water, and leaving to stand to layer, thereby obtaining an organic layer, namely, a lidocaine based dichloroethane solution; further adding hydrochloric acid into the lidocaine based dichloroethane solution, adjusting the pH value to be 3.5-4 by using hydrogen chloride, adding activated carbon to reflux for 20-40 minutes, filtering, concentrating the filtrate, cooling, crystallizing, and dying, thereby obtaining lidocaine hydrochloride. The lidocaine hydrochloride prepared by using the method is simple in synthesis process and high in product purity, that is, the purity can be greater than 99%, and the total yield is greater than 84%.
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- On-demand continuous-flow production of pharmaceuticals in a compact, reconfigurable system
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Pharmaceutical manufacturing typically uses batch processing at multiple locations. Disadvantages of this approach include long production times and the potential for supply chain disruptions. As a preliminary demonstration of an alternative approach, we report here the continuous-flow synthesis and formulation of active pharmaceutical ingredients in a compact, reconfigurable manufacturing platform. Continuous end-to-end synthesis in the refrigerator-sized [1.0 meter (width) × 0.7 meter (length) × 1.8 meter (height)] system produces sufficient quantities per day to supply hundreds to thousands of oral or topical liquid doses of diphenhydramine hydrochloride, lidocaine hydrochloride, diazepam, and fluoxetine hydrochloride that meet U.S. Pharmacopeia standards. Underlying this flexible plug-and-play approach are substantial enabling advances in continuous-flow synthesis, complex multistep sequence telescoping, reaction engineering equipment, and real-time formulation.
- Adamo, Andrea,Beingessner, Rachel L.,Behnam, Mohsen,Chen, Jie,Jamison, Timothy F.,Jensen, Klavs F.,Monbaliu, Jean-Christophe M.,Myerson, Allan S.,Revalor, Eve M.,Snead, David R.,Stelzer, Torsten,Weeranoppanant, Nopphon,Wong, Shin Yee,Zhang, Ping
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