With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1095010-47-1,1-tert-Butyl 3-methyl 5-hydroxypiperidine-1,3-dicarboxylate,as a common compound, the synthetic route is as follows.
To a dichloromethane solution (25 mL) of 1-tert-butyl 3-methyl 5-hydroxypiperidine-1,3-dicarboxylate (1.30 g), Dess-Martin reagent (2.33 g) was added. After stirring for 3 hours at room temperature, Dess-Martin reagent (1.31 g) was further added to the reaction solution, and the mixture was stirred for further 2.5 hours. Then, saturated aqueous solution of sodium hydrogen carbonate (50 mL) and a 10% sodium thiosulfate aqueous solution (50 mL) were added sequentially to the mixture, and the organic layer was separated. The product was further extracted from the aqueous layer with dichloromethane (10 mL) four times. The obtained organic layer was dried with anhydrous sodium sulfate, filtered. The filtrate was concentrated under reduced pressure, the residue was purified with silica gel column chromatography (chloroform/methanol=100/0 to 98/2) to give 1-tert-butyl 3-methyl 5-oxopiperidine-1,3-dicarboxylate (1.14 g) as an oil. 1H NMR (300 MHz, CDCl3) delta 1.46 (s, 9H), 2.58-2.79 (m, 2H), 3.03-3.11 (m, 1H), 3.73 (s, 3H), 3.77-3.93 (m, 2H), 4.02 (s, 2H)
1095010-47-1, 1095010-47-1 1-tert-Butyl 3-methyl 5-hydroxypiperidine-1,3-dicarboxylate 45790959, apiperidines compound, is more and more widely used in various fields.
Reference£º
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; SUMITOMO DAINIPPON PHARMA CO., LTD.; FUSANO, Akira; KOBAYASHI, Tomonori; SAITO, Yasuhiro; KANAI, Toshio; (55 pag.)US2016/221948; (2016); A1;,
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