反应详情

To 4-(4-chloro-7H-pyrrolo[2,3-d]pyrimidin-6-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (601.6 mg, 1.797 mmol, 1 eq), a 4.0 M solution of HCl in 1,4-dioxane (15 mL, 33 eq) was added and the reaction was stirred at rt for 18 h. The solid was then filtered off, washed several times with ether, and dried under vacuum pressure, yielding the title compound as a yellow solid. 1H NMR (400 MHz, DMSOd6): δ=2.77 (s, 2H), 3.33 (d, J=4.8 Hz, 2H), 3.83 (s, br, 2H), 5.27-5.65 (s, br, —NH+H2O), 6.60 (s, 1H), 6.71 (d, J=1.6 Hz, 1H), 8.59 (s, 1H), 9.30 (s, br, —NH), 12.85 (s, H+). MS (ES+): m/z 235.09/237.11 (3) [MH+]; 206.12/208.14 (100) [MH+—CH3N). HPLC: tR=1.52 min (ZQ2000, polar—5 min).

1. filtrationThe solid was then filtered off
2. washwashed several times with ether
3. customdried under vacuum pressure