Hydrochloric Acid → HCID 68571229, compound

Participants

Reaction Steps

tert-Butyl 4-(2-oxo-4,5-dihydro-1H-pyrido[2,3-d][1,3]diazepin-3(2H)-yl)piperidine-1-carboxylate (0.51 g, 1.472 mmol) was dissolved in dichloromethane (8 ml). Trifluoroacetic acid (2 ml, 26.0 mmol) was added to the solution. The mixture was stirred at room temperature for 4 hours. All volatiles were removed by roto-vap. Residue was dissolved in dichloromethane (10 mL). 2M Hydrogen chloride in diethyl ether (2.58 ml, 5.15 mmol) was added to the mixture. The mixture was stirred at room temperature for 15 minutes and then all volatiles were removed. The resulting off-white solid was washed with anhydrous diethyl ether four times to afford the title compound as white solid in 99% yield. 1H NMR (500 MHz, D2O) δ ppm 8.01-8.29 (m, 2 H) 7.38 (t, J=6.71 Hz, 1 H) 4.63-4.88 (m, 2 H) 4.29-4.53 (m, 1 H) 3.61-3.71 (m, 2 H) 3.45-3.62 (m, 2 H) 3.01-3.27 (m, 4 H) 1.93-2.21 (m, 4 H).

Provenance & Evidence