Hydrochloric Acid → N~1~-(Pyridin-2-yl)ethane-1,2-diamine--hydrogen chloride (1/2)

反応式

[ClH:1].C([NH:9][CH2:10][CH2:11][NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1)(OC(C)(C)C)=O>O1CCOCC1.C(Cl)Cl>[ClH:1].[ClH:1].[NH2:9][CH2:10][CH2:11][NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1

参加物

実験手順

4 N HCl in dioxane (3.2 mL) was added in a stream to a solution of 2-[[2-(Boc-amino)ethyl]amino]pyridine (148.4 mg, 0.63 mmole) in anhydrous CH2Cl2 (3.2 mL) at 0° C., then the reaction was warmed to RT. After 2 hr, the mixture was suction filtered to collect the precipitated solid, which was washed with anhydrous Et2O and dried to afford the title compound (132.8 mg, quantitative) as a yellow solid: 1H NMR (400, CD3OD) δ 7.99-8.07 (m, 1 H), 7.92-7.98 (m, 1 H), 7.19 (d, J=9.1 Hz, 1 H), 6.98-7.04 (m, 1 H), 3.76 (t, J=6.2 Hz, 2 H), 3.27 (t, J=6.2 Hz, 2 H, partially obscured by residual solvent signal); MS (ES) m/e 138 (M+H)+.