反应详情

温度

0 °C

9-(2-methoxycarbonyl-1-cyclobutyl)adenine (500 mg, 2.02 mmol) from Step A was dissolved in 250 mL of THF and the solution was cooled to 0° C. with stirring under a nitrogen atmosphere. Lithium aluminum hydride (115 mg, 3.03 mmol) was added and the reaction mixture was stirred for 30 minutes then quenched with 115 μL of water followed by 115 μL of 15% sodium hydroxide and 345 μL of water. The reaction mixture was filtered through Celite filter aid. The Celite was washed with ethyl acetate and the filtrate concentrated in vacuo to give 430 mg (97% yield) of the title compound; MS DCI-NH3M/Z: 220 (M+H)+ ; 1H NMR (d6-DMSO) δ 1.65 (m, 1H), 1.90 (m, 1H), 2.32 (m, 1H), 2.50 (m, 1H), 3.10 (m, 1H), 3.47 (t, 2H), 4.67-4.77 (m, 2H, H-1'+OH), 7.20 (bs, 2H), 8.12 (s, 1H), 8.27 (s, 1H); Analysis calculated for C10H13N5O: C, 54.78; H, 5.98; N, 31.95. Found: C, 54.79; H, 6.01; N, 31.66.

1. stirringthe reaction mixture was stirred for 30 minutes
2. customthen quenched with 115 μL of water
3. filtrationThe reaction mixture was filtered through Celite
4. filtrationfilter aid
5. washThe Celite was washed with ethyl acetate
6. concentrationthe filtrate concentrated in vacuo