反应详情

To a solution of 7-allyl-1H-purine-2,6(3H,7H)-dione (15 g, 78.13 mmol) in DMF (200 mL) was added potassium carbonate (23.7 g, 171.74 mmol), followed by dropwise addition of iodoethane (3.6 mL, 44.54 mmol). The reaction was stirred at room temperature overnight. The reaction was concentrated and partitioned between ethyl acetate and water. The organic phase was washed with brine and dried over sodium sulfate, and concentrated to give a crude product which was purified by silica gel chromatography eluting with petroleum/ethyl acetate (6:1 to 3:1) to give 7-allyl-3-ethyl-1H-purine-2,6(3H,7H)-dione (7 g, 40.7% yield) as yellow solid. LCMS retention time 0.402 min; LCMS MH+ 221.

1. concentrationThe reaction was concentrated
2. custompartitioned between ethyl acetate and water
3. washThe organic phase was washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customto give a crude product which
7. customwas purified by silica gel chromatography
8. washeluting with petroleum/ethyl acetate (6:1 to 3:1)