反应详情

Sodium borohydride (0.234 g, 6.20 mmol) was added to a solution of methyl 2-(((benzyloxy)carbonyl)amino)-3-(1,3-dimethyl-2,4-dioxo-5-phenyl-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)propanoate (1.52 g, 3.10 mmol) and lithium chloride (0.263 g, 6.20 mmol) in THF (79 ml) and EtOH (39.7 ml) at 0° C. The mixture was stirred at room temperature for 16 hours. The reaction was quenched with saturated NaHCO3(aq) (20 mL), diluted with water (50 ml) and extracted with DCM (3×150 ml). The combined organic extracts were diluted with MeOH (50 ml), dried over sodium sulfate, passed through a hydrophobic frit and evaporated under vacuum to afford the title compound and was a by-product. The resulting mixture was taken forward to the next step without further purification.

1. customThe reaction was quenched with saturated NaHCO3(aq) (20 mL)
2. additiondiluted with water (50 ml)
3. extractionextracted with DCM (3×150 ml)
4. additionThe combined organic extracts were diluted with MeOH (50 ml)
5. dry with materialdried over sodium sulfate
6. customevaporated under vacuum