反应详情

tert-Butyl (1-{4-[2-(2-methoxypyrimidin-5-yl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl]phenyl}cyclobutyl)carbamate (45 mg, 0.077 mmol) in MeOH (0.5 mL) was added 4N HCl-dioxane (2 mL) and stirred at r.t for 19 hours. The mixture was concentrated, then sat.NaHCO3 aq. was added. The mixture was extracted with CH2Cl2+MeOH (×3), dried over Na2SO4, then filtrated through Celite pad. The filtrate was concentrated and the residue was purified by preparative thin-layer chromatography (CH2Cl2/MeOH=4:1) to afford the desired product (7 mg, 18%) as a yellow solid. 1HNMR (DMSO-d6) 400 MHz δ: 8.58 (s, 1H), 8.23 (br s, 2H), 8.09 (dd, J=4.6 Hz and 1.7 Hz, 1H), 7.92 (dd, J=4.6 Hz and 1.1 Hz, 1H), 7.51 (d, J=8.6 Hz, 2H), 7.34 (td, J=8.6 Hz and 1.7 Hz, 1H), 7.28 (d, J=8.0 Hz, 1H), 7.23 (d, J=7.4 Hz, 2H), 7.10 (td, J=7.4 Hz and 1.1 Hz, 1H), 6.87 (dd, J=8.0 Hz and 1.7 Hz, 1H), 6.76 (dd, J=8.0 Hz and 4.6 Hz, 1H), 2.44-2.39 (m, 2H), 2.20-2.15 (m2H), 2.09-2.00 (m, 1H), 1.74-1.67 (m, 1H). LCMS: 474 [M+H].

1. concentrationThe mixture was concentrated
2. additionNaHCO3 aq. was added
3. extractionThe mixture was extracted with CH2Cl2+MeOH (×3)
4. dry with materialdried over Na2SO4
5. filtrationfiltrated through Celite pad
6. concentrationThe filtrate was concentrated
7. customthe residue was purified by preparative thin-layer chromatography (CH2Cl2/MeOH=4:1)