68947-43-3,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.68947-43-3,1-Methylpiperidine-4-carboxylic acid,as a common compound, the synthetic route is as follows.
A mixture of 1-methylpiperidine-4-carboxylic acid (1.72 g) obtained above, tert-butyl 2-hydroxyethyl(methyl)carbamate (1.75 g) obtained in Reference Synthetic Example 1, 1-ethyl-3-[3-(dimethylamino)propyl]carbodiimide (2.30 g), 4-dimethylaminopyridine (0.24 g) and acetonitrile (50 mL) was stirred at room temperature for 16 hrs. The reaction solution was concentrated under reduced pressure, and to the residue was added saturated aqueous solution of sodium bicarbonate (50 mL), and extracted with ethyl acetate (100 mL). The ethyl acetate layeer was washed with saturated brine (50 mL), and dried over anhydrous magnesium sulfate, followed by concentrating under reduced pressure. The residue was purified with basic silica gel column chromatography (eluted with methanol : ethyl acetate = 50 : 50, then 80 : 20). To the purified material (2.73 g) was added 1 N hydrochloric acid (25 mL), and stirred at room temperature overnight. The reaction solution was concentrated under reduced pressure, and isopropanol was added, then, concentrated again under reduced pressure. The precipitated crystals were collected by filtration to give title compound as colorless solid (1.72 g).1H-NMR (DMSO-d6) : 1.70-2.20(4H,m), 2.40-3.50 (13H,m), 4.31(2H,m), 9.25(2H,br), 10.77 (1H,br).
The synthetic route of 68947-43-3 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Takeda Pharmaceutical Company Limited; EP1602362; (2005); A1;,
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