反应详情

1-isobutyl-6-(4-methoxybenzyl)-3-methyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (1.88 g, 5.5 mmol) and hexachloroethane (6.5 g, 26.5 mmol) are dissolved in anhydrous THF (3 mL), and then 1.0 M LiHMDS in THF (11 mL, 11 mmol) is added dropwise over 2 hours. The reaction mixture is stirred at room temperature for an hour, and then quenched with saturated ammonium chloride aqueous solution. The mixture is poured into cold water (100 mL), and then extracted with ethyl acetate three times. The combined organic phase is dried with anhydrous sodium sulfate. After filtration, the filtrate is evaporated to dryness to give 2.5 g of crude product as light brown solids, which is used in the next step without further purification. MS (ESI) m/z 376.1 [M+H]+.

1. customquenched with saturated ammonium chloride aqueous solution
2. additionThe mixture is poured into cold water (100 mL)
3. extractionextracted with ethyl acetate three times
4. dry with materialThe combined organic phase is dried with anhydrous sodium sulfate
5. filtrationAfter filtration
6. customthe filtrate is evaporated to dryness