反应详情

To a stirred solution of the crude tert-butyl 6-formylpyrimidin-4-ylcarbamate (4.6 g, 0.020 mol) in MeOH (100 mL) was added sodium borohydride (0.74 g, 0.020 mol) in four portions at room temperature. After addition, the resulting mixture was stirred for 1 hour and then water (50 mL) was added. The solvent was removed under reduced pressure and the resulting aqueous residue was extracted with EtOAc (3×100 mL). The combined organic extract was washed with water (30 mL) and brine (30 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue was purified via silica gel column chromatography, eluting with DCM/MeOH (30:1) to give the desired product (1.4 g, 30% yield). LCMS (ESI) m/z: 226.0 [M+H+].

1. additionAfter addition
2. customThe solvent was removed under reduced pressure
3. extractionthe resulting aqueous residue was extracted with EtOAc (3×100 mL)
4. extractionThe combined organic extract
5. washwas washed with water (30 mL) and brine (30 mL)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified via silica gel column chromatography
9. washeluting with DCM/MeOH (30:1)