反应详情

Hydrogen chloride HCl (340 μL of a 4M solution in dioxane) was added to a solution of [(S)-1-((S)-6-fluoro-3-methyl-3,4-dihydro-5-oxa-1,2a-diazaacenaphthylen-2-yl)ethyl][9-(tetrahydropyran-2-yl)-9H-purin-6-yl]amine (117 mg, 0.27 mmol) in MeOH (1 mL) and the reaction was stirred at RT for 30 min. The crude reaction mixture was passed through a 2 g Isolute® SCX-2 cartridge, eluting with 2M NH3/MeOH. The basic fraction was concentrated in vacuo to give 441 (88 mg, 92%) as an off-white solid. LCMS (Method K): RT 2.61 min [M+H]+ 354.0. 1H NMR (CD3OD, 400 MHz): δ 8.23 (1H, s), 8.05 (1H, s), 7.08 (1H, dd, J=8.8, 3.1 Hz), 6.93 (1H, dd, J=12.1, 8.8 Hz), 5.77 (1H, br s), 5.19 (1H, qdd, J=6.7, 2.6, 1.8 Hz), 4.48 (1H, dd, J=11.5, 1.8 Hz), 4.20 (1H, dd, J=11.5, 2.6 Hz), 1.80 (3H, d, J=7.0 Hz), 1.47 (3H, d, J=6.7 Hz)

1. customThe crude reaction mixture
2. washeluting with 2M NH3/MeOH
3. concentrationThe basic fraction was concentrated in vacuo