反应详情

温度

45 °C

A 4.0 M solution of HCl in 1,4-dioxane (100 ml) was added to a solution of [1-(2-cyano-1-methyl-ethyl)-piperidin-4-yl]-carbamic acid tert-butyl ester (50.0 mmol) in 1,4-dioxane (50 ml) at 25° C. The reaction mixture was stirred at 45° C. for 3.5 h, then was cooled to 25° C. and concentrated under reduced pressure to afford crude 3-(4-amino-piperidin-1-yl)-butyronitrile (hydrochloride salt) as a beige solid. 1H NMR (400 MHz, DMSO) δ 8.52 (s, 2H), 4.21 (s, 2H), 3.83-3.68 (m, 1H), 3.49-3.25 (m, 2H), 3.17 (dd, J=16.9, 8.0 Hz, 1H), 2.23-1.99 (m, 2H), 1.42 (d, J=6.7 Hz, 1H). This material was used in the next step below without additional purification or characterization.

1. temperaturewas cooled to 25° C.
2. concentrationconcentrated under reduced pressure