反应详情

To a solution of tert-butyl [5-(2-{5-(aminomethyl)-2-[(tert-butoxycarbonyl)amino]phenyl}ethyl)pyridin-3-yl]carbamate (0.81 g, 1.8 mmol) and 2,4,5-trichloropyrimidine (0.45 g, 2.4 mmol) in N,N-dimethylformamide (10 mL) was added potassium carbonate (1.30 g, 9.37 mmol). The resultant mixture was stirred overnight at 45° C. The reaction was quenched with water. EtOAc was added and the layers were separated. The aqueous layer was extracted with EtOAc once. The combined organic layers were washed with water, and then dried (Na2SO4), filtered, and concentrated under vacuum. The crude product was purified by silica gel column chromatography to give the desired product as a white powder (0.44 g, 40%). LCMS for C28H35Cl2N6O4 (M+H)+: m/z=589.1, 591.1.

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