Hydrochloric Acid → (6-(1,4-Diazepan-1-yl)pyridin-2-yl)(2-amino-5-bromopyridin-3-yl)methanone

関与物質

反応手順

To a suspension of tert-butyl 4-(6-(2-amino-5-bromonicotinoyl)pyridin-2-yl)-1,4-diazepane-1-carboxylate (0.050 g, 0.10 mmol) in 1,4-dioxane (2 ml) was added 4 M HCl in 1,4-dioxane (1 ml) and the resulting mixture was stirred at room temperature for 5 hours. Reaction mixture was then concentrated to dryness in vacuo and the crude product purified by prep-LCMS, then freeze-dried to leave title compound as a yellow solid (13.5 mg, 36%). 1H NMR (DMSO-d6 1.84-1.76 (2H, m), 2.08 (1H, s), 2.71-2.68 (1H, m), 2.89-2.86 (1H, m), 3.72-3.28 (6H, masked signal), 6.89 (10.5H, d), 6.95 (0.5H, d), 7.05 (0.5H, d), 7.10 (0.5H, d), 7.74-7.68 (1H, m), 7.81 (2H, br s), 8.31 (1H, d), 8.54 (1H, d). ES+ 378.15.

情報源と証拠