2,8-Diazaspiro[4.5]decan-1-one, hydrochloride (1:1) synthesis

Yield:-

Reaction Conditions:

in dichloromethane;water at 20; for 8 h;

Steps:

A Step A: 2,8-diazaspiro[4.Sldecan-1-one hydrochloride:
Step A: 2,8-diazaspiro[4.Sldecan-1-one hydrochloride: To a solution of tert-butyl 1-oxo-2,8- diazaspiro[4.5]decane-8-carboxylate (Inermediate 14, 92 g, 0.36 mol) in CH2C12 (1 L) was slowly added a 4 M HC1 solution (500 mL). The mixture was stirred for 8 h at RT. The mixture was concentrated under vacuum to afford the title compound. ‘H NMR (400 MHz, DMSO-d6) ö 9.35 (s, 1H), 9.02 (s, 1H), 7.72 (s, 1H), 3.30-3.20 (m, 2H), 3.16 (m,J= 6.8Hz, 2H), 2.98-2.85(m, 2H), 1.96 (m,J= 6.8Hz, 2H), 1.90-1.80 (m, 2H), 1.55 (d,J 14Hz, 2H).

References:

MERCK SHARP & DOHME CORP;TANG, Haifeng;PIO, Barbara;JIANG, Jinlong;PASTERNAK, Alexander;DONG, Shuzhi;FERGUSON, Ronald Dale, II;GUO, Zack Zhiqiang;CHOBANIAN, Harry;FRIE, Jessica;GUO, Yan;WU, Zhicai;YU, Yang;WANG, Ming WO2015/17305, 2015, A1 Location in patent:Page/Page column 106