反应详情

To a solution of tert-butyl [3-(2-{5-amino-2-[(tert-butoxycarbonyl)amino]phenyl}ethyl)phenyl]carbamate (0.4 g, 0.9 mmol) and 2,4-dichloro-5-fluoropyrimidine (0.156 g, 0.936 mmol) in N,N-dimethylformamide (7 mL) was added potassium carbonate (0.662 g, 4.79 mmol). The resultant mixture was stirred overnight at rt overnight. The reaction was quenched with water. EtOAc was added and the layers were separated. The aqueous layer was extracted with EtOAc twice. The combined organic layers were washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified by silica gel column chromatography to give the desired product (0.32 g, 61%). LCMS for C28H33ClFNaN5O4 (M+Na)+: m/z=580.2.

1. customThe reaction was quenched with water
2. additionEtOAc was added
3. customthe layers were separated
4. extractionThe aqueous layer was extracted with EtOAc twice
5. washThe combined organic layers were washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified by silica gel column chromatography