反应详情

3-[Benzyloxycarbonyl-(1,3-dimethyl-2,4-dioxo-5-phenyl-1,2,3,4-tetrahydro-pyrrolo[3,4-d]pyrimidin-6-yl)-amino]-propionic acid (step 3) (1.09 g, 2.288 mmol) and Polyphosphoric acid (3 g, 2.288 mmol) were heated together at 100° C. (block temp) for 30 mins. The reaction mixture was cooled to RT and the residue dissolved in minimum volume of water. The mixture was basified by slow addition of 2M NaOH(aq), and extracted with chloroform (4×). The combined organic extracts were passed through a hydrophobic frit and evaporated under reduced pressure. Purification of the residue by chromatography on silica, eluting with MeOH/DCM afforded the title compound as a white solid.

1. extractionextracted with chloroform (4×)
2. customevaporated under reduced pressure
3. customPurification of the residue by chromatography on silica
4. washeluting with MeOH/DCM