反应详情

To a solution of tert-butyl 2-methoxyethyl((4-oxo-4,5,7,8-tetrahydro-3H-pyrano[4,3-d]pyrimidin-2-yl)methyl)carbamate (257 mg, 0.545 mmol) in dioxane (5 mL) was added hydrochloric acid (4M in dioxane, 0.818 mL, 3.3 mmol) and the solution was stirred for 8 h. The precipitate was filtered and washed with ether. The residue was re-dissolved in ether, and stirred overnight (8 h) in ether. The precipitate was filtered and washed with ether to yield the title compound as a hydrochloride salt (107 mg). 1H NMR (400 MHz, MeOD) δ ppm 4.50 (s, 2H) 4.27 (s, 2H) 3.90-4.03 (m, 3H) 3.66-3.77 (m, 2H) 3.43 (s, 3H) 3.35-3.41 (m, 3H) 2.74 (s, 2H). MS (m/z, MH+): 239.3

1. filtrationThe precipitate was filtered
2. washwashed with ether
3. dissolutionThe residue was re-dissolved in ether
4. stirringstirred overnight (8 h) in ether
5. filtrationThe precipitate was filtered
6. washwashed with ether