1,4-Dioxane hydrochloride → HCID 67502938, compound

Participants

Reaction Steps

tert-Butyl {1-[4-(2-{4-[(methylsulfonyl)amino]phenyl}-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]cyclobutyl}carbamate (30.9 mg, 0.0476 mmol) was dissolved in DCM (1 mL). 4M HCl/dioxane (1 mL) was added to the mixture and stirred at room temperature for 13.5 hours. The mixture was concentrated and solidified with ether. The precipitated solids were collected by filtration and washed with ether to afford desired product (24.4 mg, 77.9%) as pale yellow solid. 1HNMR (DMSO-d6) 400 MHz δ: 9.90 (s, 1H), 8.76 (br s, 2H), 8.67 (s, 1H), 8.12 (dd, J=4.8, 1.6 Hz, 1H), 7.95 (dd, J=8.0, 1.6 Hz, 1H), 7.59-7.53 (m, 2H), 7.49-7.45 (m, 2H), 7.43-7.37 (m, 1H), 7.36-7.29 (m, 3H), 7.18-7.11 (m, 3H), 6.90 (dd, J=8.0, 1.6 Hz, 1H), 6.76 (dd, J=8.0, 4.8 Hz, 1H), 3.02 (s, 3H), 2.62-2.53 (m, 4H), 2.27-2.13 (m, 1H), 1.88-1.75 (m, 1H); LCMS: 549 [M+H].

Provenance & Evidence