反应详情

温度

75 °C

7-Benzyl-3,8-dimethylxanthine (500 mg, 1.85 mmol) was added to a suspension of sodium hydride (50.5 mg) in anhydrous DMSO (20 ml) and stirred for 30 min. (R)-5-acetoxy-1-chlorohexane (357 mg) (prepared according to Kline et al. U.S. Pat. No. 5,629,423 (1997)) was added and the mixture was heated at 70-80° C. for 12 h. After cooling to room temperature, the reaction was quenched by the addition of water (50 ml) and extracted with ethyl acetate (3×75 ml). The combined extracts were washed with water (2×50 ml), with saturated aqueous sodium chloride solution (50 ml), dried over magnesium sulfate and concentrated. The product was purified by flash chromatography (silica gel) eluting with ethyl acetate. Yield=638 mg.

1. customprepared
2. addition5,629,423 (1997)) was added
3. temperatureAfter cooling to room temperature
4. customthe reaction was quenched by the addition of water (50 ml)
5. extractionextracted with ethyl acetate (3×75 ml)
6. washThe combined extracts were washed with water (2×50 ml), with saturated aqueous sodium chloride solution (50 ml)
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated
9. customThe product was purified by flash chromatography (silica gel)
10. washeluting with ethyl acetate