With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.56839-43-1,1-(4-Ethylphenyl)-2-methyl-3-(piperidin-1-yl)propan-1-one hydrochloride,as a common compound, the synthetic route is as follows.
56839-43-1, Example 1 – Preparation of substantially enantiopure crystalline hydrochloride salts of eperisone[0082] Raceniic eperisone hydrochloride was separated into substantially enantiopure fractions of eperisone free base using ehiral chromatography. The isocratic supercritical fluid chromatography method used a mobile phase composed of liquid CO2 with a 5% eosolvent mixture of 50:50 methanol :isopropanol containing 2% isopropylamine. The column was a Chiralpak AD-H in a 3.0 x 25 cm format with a total mobile phase flow of 80 g/minute. Chromatography of 51.1 g of racemic eperisone hydrochloride afforded solutions of two fractions (Fraction 1 was earlier eluting; Fraction 2 was later eluting). Each solution was dried by rotary evaporation to give solids of each substantially pure enantiomer as the free base. Contaminating isopropylamine was removed from each fraction by adding acetonitrile to the solid and drying by rotary evaporation to remove the acetonitrile-isopropylamine azeotrope and acetonitrile. Each fraction consisted of white, waxy solids, which were dissolved in acetonitrile. Each acetonitrile solution was cooled with stirring in an ice bath and treated with a slowly bubbled stream of hydrochloride gas for 5 minutes. Rotary evaporation to remove acetonitrile yielded substantially pure, crystalline eperisone hydrochloride of each enantiomer as white powders. The yield of each fraction and enantiomeric purity of each fraction as determined by ehiral HPLC are shown in the following table;Analytical data were obtained on the final products: the XRPD patterns were as shown in FIGS. IA and IB, the DSC thermogram was as shown in FIG. 4, the 1H-NMR spectrum was as shown in FIGS. 7A-7G, the TGA profile was as shown in FIG. 10, and the Raman spectra were as shown in FIGS. 13A and 13B. In aeetonitrile, the solubility of the substantially enantiopure crystalline eperisone hydrochloride was determined to be greater than 11 mg/mL, calculated based on the total solvent used to give a solution. The optical rotation of substantially enantiopure eperisone hydrochloride fraction Fl was measured and the specific rotation calculated: (c 1.05, aeetonitrile). The optical rotation of substantially enantiopure eperisone hydrochloride fraction F2 was measured and the specific rotation calculated: (c 1.05, aeetonitrile).
56839-43-1 1-(4-Ethylphenyl)-2-methyl-3-(piperidin-1-yl)propan-1-one hydrochloride 123698, apiperidines compound, is more and more widely used in various fields.
Reference：
Patent; BIONEVIA PHARMACEUTICALS, INC.; KALOFONOS, Isabel; STAHLY, G., Patrick; MARTIN-DOYLE, William; KALOFONOS, Dimitris; HANKO, Jason, A.; STULTS, Jeffrey, S.; KIPLINGER, Jeffrey, P.; WO2010/17135; (2010); A2;,
Piperidine – Wikipedia
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