反应详情

To a solution of 7-(4-chlorobenzyl)-1H-purine-2,6(3H,7H)-dione (2.2 g, 7.97 mmol) in THF (30 mL) was added NCS (1.1 g, 8.27 mmol) at 0° C. in portions. Then the resulting mixture was stirred at room temperature until it became a clear solution. The reaction was immediately quenched with ice-water and concentrated. The residue was extracted with ethyl acetate. The organic phase was washed with saturated sodium bicarbonate and brine, dried over sodium sulfate, and concentrated to give a crude product. This material was purified by silica gel chromatography eluting with DCM/methanol (50:1 to 20:1) to give 8-chloro-7-(4-chlorobenzyl)-1H-purine-2,6(3H,7H)-dione (450 mg, 18.2% yield) as white solid. LCMS retention time 1.071; LCMS MH+-58 311.

1. customThe reaction was immediately quenched with ice-water
2. concentrationconcentrated
3. extractionThe residue was extracted with ethyl acetate
4. washThe organic phase was washed with saturated sodium bicarbonate and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customto give a crude product
8. customThis material was purified by silica gel chromatography
9. washeluting with DCM/methanol (50:1 to 20:1)