Hydrochloric Acid → 11-Amino-1-piperzin-1-yl-undecane-1-one dihydrochloride salt

Participants

Reaction Conditions

Reaction Steps

A solution of 4.0 M hydrochloric acid in dioxane (1 mL) was added dropwise to a solution of amide 7 (204 mg, 0.43 mmol) in dichloromethane (3 mL) which had been pre-cooled to 0° C. The reaction was allowed to warm to ambient temperature, stirred for 2 hours, and the solvent then removed under vacuum. Recrystallization from methanol and diethyl ether produced salt 8 (123 mg, 84%) as a white solid: 1H NMR (300 MHz, CD3OD) δ 1.34 (s, 12H), 1.58-1.66 (m, 4H), 2.43 (t, 2H, J=7.4 Hz), 2.90 (t, 2H, J=7.5 Hz), 3.20-3.28 (m, 4H), 3.78-3.83 (m, 4H); m/z (ESI) 270 [C15H31N3O+H]+.

Provenance & Evidence