反应详情

{2-[5-(3-Chloro-phenyl)-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydro-pyrrolo[3,4-d]pyrimidin-6-yl]-ethyl}-carbamic acid tert-butyl ester (step 5) (429 mg, 0.991 mmol) was dissolved in DCM (10 ml). TFA (1.374 ml, 17.84 mmol) was charged in 2 portions and the reaction stirred under nitrogen. After 2 hrs, the pH of the mixture was adjusted to pH 11 with saturated K3CO3 solution (20 mL). The layers were separated and the aqueous extracted with DCM (4×20 mL). The combined organics were passed through a hydrophobic frit and evaporated under reduced pressure to afford a tan solid, which was dried under vacuum at 50° C. for 5 h to afford the title compound as a tan solid.

1. customThe layers were separated
2. extractionthe aqueous extracted with DCM (4×20 mL)
3. customevaporated under reduced pressure
4. customto afford a tan solid, which
5. customwas dried under vacuum at 50° C. for 5 h