反应详情

Et3N (29.3 μL, 0.260 mmol) and phenyl isocyanate (8.0 μL, 0.0771 mmol) were added to a solution of tert-butyl (1-{4-[2-(3-aminophenyl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl]phenyl}cyclobutyl)carbamate (40.0 mg, 0.0701 mmol) in DCM (1 mL) at 0° C., and stirred at room temperature. After reaction was completed, the mixture was diluted with sat. NaHCO3 and extracted with CHCl3 (3×). The combined organic layers were dried over anhydrous Na2SO4, and concentrated. The residue was purified by PTLC (CHCl3/MeOH=9:1) to afford desired product (35.4 mg, 69.3%) as white solid. 1HNMR (DMSO-d6) 400 MHz δ: 8.15 (dd, J=7.8, 1.4 Hz, 1H), 8.05 (dd, J=4.6, 1.8 Hz, 1H), 7.90-6.59 (m, 20H), 6.30 (s, 1H), 6.18-5.38 (m, 1H), 2.67-2.54 (m, 2H), 2.52-2.39 (m, 2H), 2.25-2.10 (m, 1H), 2.06-1.86 (m, 1H), 1.37 (s, 9H).

1. customAfter reaction
2. extractionextracted with CHCl3 (3×)
3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
4. concentrationconcentrated
5. customThe residue was purified by PTLC (CHCl3/MeOH=9:1)