反应详情

Hydrogen chloride, HCl (384 μL of a 4M solution in dioxane) was added to a solution of [1-(6-fluoro-3,4-dihydro-5-oxa-1,2a-diazaacenaphthylen-2-yl)ethyl]-[9-(tetrahydropyran-2-yl)-9H-purin-6-yl]amine (130 mg, 0.31 mmol) in MeOH (1 mL) and the reaction was stirred at RT for 20 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 435 (92 mg, 87%) as a pale yellow solid. LCMS (Method K): RT 2.28 min [M+H]+ 340.0. 1H NMR (CD3OD, 400 MHz): δ 8.22 (1H, s), 8.06 (1H, s), 7.06 (1H, dd, J=8.9, 3.1 Hz), 6.91 (1H, dd, J=12.0, 8.9 Hz), 5.78 (1H, br s), 4.63-4.38 (4H, m), 1.79 (3H, d, J=7.0 Hz)

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