3-Ethynylpiperidine hydrochloride synthesis

Yield: 86%

Reaction Conditions:

with hydrogenchloride in 1,4-dioxane at 20; for 16 h;

Steps:

INTERMEDIATE 35 (METHOD V); 3-Ethynylpiperidine hydrochloride; To Intermediate 33 (1.50 g, 7.18 mmol) was added HCl (4iVm dioxane, 50 mL). The reaction mixture was stirred at r.t. for 16 h and concentrated in vacuo. Trituration with Et₂O gave the title compound (0.91 g, 86%). δ_H (DMSOd₆) 9.02 (2H, br. s), 3.38- 3.24 (IH, m), 3.21-3.08 (2H, m), 2.94-2.76 (3H, m), 2.00-1.87 (IH, m), 1.83-1.73 (IH, m), 1.73-1.60 (IH, m), 1.60-1.48 (IH, m).

References:

UCB PHARMA S.A. WO2007/141504, 2007, A1 Location in patent:Page/Page column 59