反应详情

A solution of 1-(3-((((3aR,4R,6R,6aR)-6-(6-amino-9H-purin-9-yl)-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl)methyl)(methyl)amino)cyclobutyl)-3-(4-(tert-butyl)phenyl)urea (125 mg, 0.23 mmol) in TFA (0.90 mL) and 0.10 mL of water were stirred for 1 hour at room temperature. The reaction was concentrated to dryness, dissolved in MeOH (5 mL) and K2CO3 (60 mg) in 0.5 mL of water was added dropwise. The reaction was stirred at rt for 0.5 h and concentrated to obtain the residue which was purified by prep-TLC (DCM:MeOH:NH4OH=300:30:8, V/V) to obtain the desired compound (75 mg, Yield: 65%) as pale white solid. 1H NMR (500 MHz, MeOD): δH 8.27 (s, 1H), 8.21 (s, 1H), 7.28-7.20 (m, 4H), 6.00-5.99 (m, 1H), 4.77-4.75 (m, 1H), 4.28-4.23 (m, 2H), 3.92-3.88 (m, 1H), 2.92 (brs, 1H), 2.83-2.81 (m, 2H), 2.59-2.56 (m, 2H), 2.32 (s, 3H), 1.74-1.64 (m, 2H), 1.27 (s, 9H) ppm; ESI-MS (m/z): 525.3 [M+1]+.

1. concentrationThe reaction was concentrated to dryness
2. dissolutiondissolved in MeOH (5 mL)
3. additionK2CO3 (60 mg) in 0.5 mL of water was added dropwise
4. concentrationconcentrated
5. customto obtain the residue which
6. customwas purified by prep-TLC (DCM:MeOH:NH4OH=300:30:8, V/V)