Hydrochloric Acid → HCID 131734882, compound

Participants

Reaction Steps

To a solution of compound (S)-tert-butyl 3-(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)piperidine-1-carboxylate (3.4 g, 7.2 mmol) in dioxane (20 mL) at 0° C., a solution of HCl in dioxane (50 mL) was added until the pH was acidic at 0° C. and stirred for 30 min. at the same temperature. The reaction mixture was concentrated in vacuo to give a residue that was triturated with ether to give (S)—N-(piperidin-3-yl)-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine hydrochloride (2 g, 74%) as a free flowing solid. 1H NMR (400 MHz, DMSO-d6): δ 9.19 (s, 1H), 8.32 (s, 1H), 7.98 (d, J=8.2 Hz, 2H), 7.62 (d, J=2.5 Hz, 1H), 7.42 (d, J=8.2 Hz, 2H), 7.22 (d, J=2.5 Hz, 1H), 5.80 (s, 1H), 4.29-4.25 (m, 2H), 3.38-3.32 (m, 1H), 3.19-3.12 (m, 1H), 3.00-2.97 (m, 1H), 2.35 (s, 3H), 2.01-1.95 (m, 2H), 1.75-1.69 (m, 2H). LC-MS: m/z [M+1]=372.

Provenance & Evidence