Hydrochloric Acid → HCID 66601607, compound

Participants

Reaction Conditions

Reaction Steps

Add t-Butyl 4-(2-(4-hydroxypiperidin-1-yl)pyridin-3-yl)piperazine-1-carboxylate (306.5 g, 0.846 mol) to a 12-liter flask, followed by methanol (613 ml) and toluene (3.06 L). Stir the mixture to give a solution and then add the methanolic HCl solution (579 mL). Heat the solution to 35° C. for 2 hr. followed by 4 hr. at ambient temperature. Filter off the resulting crystalline product, wash the crystals with toluene, and then dry in a vacuum oven at 40-45° C. to provide 1-(3-(piperazin-1-yl)pyridin-2-yl)piperidin-4-ol dihydrochloride as a crystalline solid (283.5 g, 99.47%). 1H NMR 300 MHz (DMSO) δ 9.624 (bs, 2H) 7.890 (dd, J=6.4 Hz, 1H), 7.633 (d, J=7.75 Hz, 1H), 7.137 (m, 1H), 3.916 (bm, 2H), 3.727 (bm, 1H), 3.236 (bs, 9H), 1.877 (bm, 2H), 1.515 (bm, 2H).

Provenance & Evidence