反应详情

A solution of ethyl 2-(6-fluoro-1H-benzo[d]imidazol-1-yl)-8-oxo-9-(tetrahydro-2H-pyran-4-yl)-8,9-dihydro-7H-purine-6-carboxylate (600 mg, 1.41 mmol) in concentrated aqueous HCl (15 mL) was heated at 100° C. for 6 h. The mixture was concentrated and the residue triturated with diethyl ether. The solid formed was filtered and dried to give 7 as an off white solid. Yield: 410 mg, 73%. 1H NMR (400 MHz, DMSO-d6) δ, ppm: 11.84 (s, 1H), 9.20 (s, 1H), 8.47 (dd, J=2.4, 2.4 Hz, 1H), 7.82 (dd, J=5.2, 4.8 Hz, 1H), 7.26 (m, 1H), 4.63 (m, 1H), 4.04 (q, J=3.6 Hz, 2H), 3.51 (t, J=11.6 Hz, 2H), 2.60-2.54 (m, 2H), 1.80 (d, J=9.8 Hz, 2H); LCMS (EI) m/z 399 (MH)+.

1. concentrationThe mixture was concentrated
2. customthe residue triturated with diethyl ether
3. customThe solid formed
4. filtrationwas filtered
5. customdried
6. customto give 7 as an off white solid