反应详情

Example 8a (50 mg, 0.10 mmol) was reacted with imidazole (8.0 eq.) as described under General Procedure G and the crude mixture was dissolved in DCM and HCl gas was bubbled through it for 3 minutes. Then, solvent was removed under vacuum and the residue was suspended in dry ether and triturated to afford the title compound as a off-white solid (22 mg, 45%). 1H NMR (300 MHz, CDCl3) δ 9.57 (bs, 1H), 7.33 (bs, 1H) 7.19-7.14 (m, 3H), 7.02-6.96 (m, 2H), 4.60 (bs, 2H), 4.37 (bs, 2H), 3.89-3.76 (m, 5H), 2.88-2.93 (m, 1H), 2.32 (s, 3H), 2.16 (s, 3H), 1.94-1.96 (m, 2H), 1.27 (d, J=6.6 Hz, 3H). MS (ES+) m/z 475.2 (M+H+).

1. customHCl gas was bubbled through it for 3 minutes
2. customThen, solvent was removed under vacuum
3. customtriturated