1,4-Dioxane hydrochloride → HCID 67540515, compound

Participants

Reaction Steps

To a solution of (2R)-2-Boc-amino-3-(4-chlorophenyl)-1-[4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperazin-1-yl]-propan-1-one in 1 mL dioxane was added 1 mL 4M HCl/dioxane. The resulting suspension was stirred at room temperature overnight, after which it was concentrated to dryness. The solids were dissolved in minimal MeOH and then triturated with ether. The resulting solids were isolated by filtration through a flitted funnel with nitrogen pressure, rinsed with ether, and dried in vacuo to give (2R)-2-amino-3-(4-chlorophenyl)-1-[4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperazin-1-yl]-propan-1-one dihydrochloride (19 mg, 38%) as a pink powder. 1H NMR (D2O, 400 MHz) δ 8.16 (1H, s), 7.27 (1H, s), 7.18-7.11 (4H, m), 6.68 (1H, s), 4.60-4.56 (1H, m), 3.98-3.69 (4H, m), 3.61-3.52 (2H, m), 3.45-3.37 (1H, m), 3.20-3.12 (1H, m), 3.00-2.91 (2H, m). LCMS (APCI+) m/z 385 [M+H]+. HPLC Rt 1.68 min.

Provenance & Evidence