反应详情

[2-(1,3-Dimethyl-2,4-dioxo-5-phenyl-1,2,3,4-tetrahydro-pyrrolo[3,4-d]pyrimidin-6-yl)-ethyl]-carbamic acid tert-butyl ester (step 4) (1.11 g, 2.79 mmol) was dissolved in DCM (10 mL) and treated with trifluoroacetic acid (2.1 mL, 25.1 mmol). The reaction was stirred at RT for 4 h. The reaction was quenched by pouring into stirring 2M NaOH and further NaOH added until alkaline to pH paper. The layers were separated and the aqueous phase extracted with DCM (3×75 mL). The combined organic phases were washed with water (100 mL), brine (75 mL) and passed through a hydrophobic frit. The solvent was removed under reduced pressure, affording the title compound as an off-white solid.

1. customThe reaction was quenched
2. additionby pouring
3. stirringinto stirring 2M NaOH and further NaOH
4. additionadded until alkaline
5. customThe layers were separated
6. extractionthe aqueous phase extracted with DCM (3×75 mL)
7. washThe combined organic phases were washed with water (100 mL), brine (75 mL)
8. customThe solvent was removed under reduced pressure