反应详情

温度

80 °C

A stirring mixture of 2-propen-1-yl {3-[bromo(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}carbamate (6.1 g, 14.23 mmol) and 2,2-dimethylpropanamide (2.16 g, 21.35 mmol) in DMA (200 ml) was heated to 80° C. for 2 days. Upon cooling, the reaction mixture was poured into water (500 ml) and extracted with EtOAc (100 ml×5). The combined organic layers were washed with brine, separated, dried over Na2SO4, filtered, and concentrated. The crude product was added to a silica gel column and eluted with petroleum ether with EtOAc (10% to 16%) and collected fractions to obtain title compound as yellow solid (1.21 g, 19%). MS (ES): 431 [M+H]+.

1. temperatureUpon cooling
2. extractionextracted with EtOAc (100 ml×5)
3. washThe combined organic layers were washed with brine
4. customseparated
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. additionThe crude product was added to a silica gel column
9. washeluted with petroleum ether with EtOAc (10% to 16%)
10. customcollected fractions