反应详情

(R)-3-(7-Methyl-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-5-yl)-1-oxo-1-(4-(piperidin-1-yl)piperidin-1-yl)propan-2-yl 4-(7-fluoro-2-oxo-1,2-dihydroquinazolin-3(4H)-yl)piperidine-1-carboxylate (93 mg, 0.12 mmol) was dissolved in trifluoroacetic acid (50% in dichloromethane, 6 mL) and stirred at room temperature for 2 h. The reaction was concentrated and purified by column chromatography (5:95:1 to 10:90:1 methanol/dichloromethane/triethylamine). The residue was dissolved in 10% methanol/dichloromethane and passed through a plug of basic alumina to give 41 mg (53%) as a white powder. 1H-NMR (CD3OD, 500 MHz) δ −0.38-0.15 (m, 0.7H), 0.60-0.95 (m, 1H), 1.18-2.18 (m, 17H), 2.29 (m, 0.7H), 2.35-2.50 (m, 3H), 2.58-3.01 (m, 3.4H), 3.01-3.25 (m, 2.4H), 3.65-4.60 (m, 7H), 5.47 (m, 0.4H), 5.55 (dd, J=9.5, 6.1, 0.7H), 6.51 (m, 0.8H), 6.62 (m, 0.8H), 6.90-7.20 (m, 2.2H), 7.45 (bs, 1.1H), 7.98 (bs, 1H). Mass spec.: 648.64 (MH)+.

1. concentrationThe reaction was concentrated
2. custompurified by column chromatography (5:95:1 to 10:90:1 methanol/dichloromethane/triethylamine)
3. dissolutionThe residue was dissolved in 10% methanol/dichloromethane
4. customto give 41 mg (53%) as a white powder