反应详情

To a solution of (3-hydroxy-cyclobutyl)-carbamic acid tert-butyl ester (2.5 g, 13.3 mmol) in THF (40 mL) were added Cs2CO3 (8.6 g, 26.6 mmol) and 5-bromo-2,4-dichloro-pyrimidine (3 g, 13.3 mmol). The reaction mixture was heated at reflux overnight. The reaction mixture was filtered and concentrated, diluted with EtOAc and water. The aqueous phase was extracted with EtOAc (3×100 mL) and the combined organic extracts were washed with brine (60 mL), dried over MgSO4, filtered, and concentrated. Purification by flash column chromatography on silica gel to give the product (4.75 g, 12.6 mmol, yield: 95%). ESI-MS (M+1): 378 calc. for C13H17BrClN3O3 377.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. filtrationThe reaction mixture was filtered
4. concentrationconcentrated
5. additiondiluted with EtOAc and water
6. extractionThe aqueous phase was extracted with EtOAc (3×100 mL)
7. washthe combined organic extracts were washed with brine (60 mL)
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated
11. customPurification by flash column chromatography on silica gel