反应详情

温度

60 °C

N2-Butyl-8-(methyloxy)-3H-purine-2,6-diamine (157 mg, 0.447 mmol) was heated in dry DMF (3 ml) with potassium carbonate (232 mg, 1.675 mmol) at 60° C. for one hour. (3S)-3-(2-Bromoethyl)tetrahydrofuran (100 mg, 0.558 mmol) in dry DMF (2 ml) was added and the mixture stirred and heated to 60° C. under nitrogen for 4 hours. The mixture was cooled to room temperature, quenched into water (40 ml) and extracted with ethyl acetate (3×25 ml). The organic extracts were combined, dried by passage through a hydrophobic frit and concentrated under vacuum. The residue was dissolved in 1:1 MeOH:DMSO and purified by mass directed autopreparation. The desired fractions were combined and concentrated using a nitrogen blowdown unit to give the title compound as a white solid (119 mg).

1. temperatureThe mixture was cooled to room temperature
2. customquenched into water (40 ml)
3. extractionextracted with ethyl acetate (3×25 ml)
4. customdried by passage through a hydrophobic frit
5. concentrationconcentrated under vacuum
6. dissolutionThe residue was dissolved in 1:1 MeOH
7. customDMSO and purified by mass
8. concentrationconcentrated