New learning discoveries about 888952-55-4

888952-55-4 Methyl 1-Boc-3-methylpiperidine-3-carboxylate 46911995, apiperidines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.888952-55-4,Methyl 1-Boc-3-methylpiperidine-3-carboxylate,as a common compound, the synthetic route is as follows.

Example 2 – Preparation of Intermediate 2 The synthesis of Intermediate 2 followed the procedure of General Procedure 2 following. Intermediate 1 Intermediate 2 To a cold solution (-78C) of acetonitrile (1.67 g, 40.8 mmol, 1.5 eq) in tetrahydrofuran (70 mL) was added n-BuLi (23% in hexane, 2.61 g, 40.8 mmol, 1.5 eq) under inert N2 atmosphere over a period of 20 minutes. After completion of addition, the reaction was stirred for another 60 minutes. To the cold (-78C) mixture was then added Intermediate 1 (7.0 g, 27.2 mmol, 1.0 eq) in portions, and the reaction mixture was stirred for 3 hours. The reaction mixture was quenched with saturated ammonium chloride solution and the product was extracted with ethyl acetate. The organic phase was dried with sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography using silica gel (60-120 mesh size) eluting with 10-40% ethyl acetate in n-hexane, yielding product tert-butyl 3-(2- cyanoacetyl)-3-methylpiperidine-1-carboxylate (Intermediate 2; 4.775 g, yield: 65.9%) m/z 211.0 [M-56]+ 1H NMR (400 MHz, DMSO) delta 4.26 (q, J = 20.1 Hz, 2H), 3.74 (d, J = 12.6 Hz, 1H), 3.38-3.32 (m, 1H), 3.21- 3.06 (m, 2H), 1.94- 1.77 (m, 1H), 1.56- 1.31 (m, 12H), 1.06 (s, 3H) ppm., 888952-55-4

888952-55-4 Methyl 1-Boc-3-methylpiperidine-3-carboxylate 46911995, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; VERSEON CORPORATION; SHORT, Kevin Michael; ESTIARTE-MARTINEZ, Maria de los Angeles; KITA, David Ben; SHIAU, Timothy Philip; (340 pag.)WO2016/138532; (2016); A1;,
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