反应详情

NaH (0.068 g in 60% oil dispersion, 1.7 mmol) was added to a solution of compound 16 (0.180 g, 1.8 mmol) in DMF (6 mL) with stirring at room temperature. The mixture was stirred for 15 min and a solution of 4′-fluoroacetophenone (0.215 g, 1.56 mmol) in DMF (2 mL) was added. The reaction mixture was heated at 80° C. for 1 h, and then cooled, diluted with water, and extracted with EtOAc. The organic layer was washed with brine, dried, and evaporated to a yellow solid. Compound 17 crystallized to form white color needles upon standing at room temperature. The yield was 0.270 g, 67%. The structure was confirmed by 1H NMR in CDCl3. LC-MS: [M+1]=215. Purity was >98%.

1. stirringThe mixture was stirred for 15 min
2. temperatureThe reaction mixture was heated at 80° C. for 1 h
3. temperaturecooled
4. extractionextracted with EtOAc
5. washThe organic layer was washed with brine
6. customdried
7. customevaporated to a yellow solid
8. customCompound 17 crystallized
9. customto form white color needles
10. customupon standing at room temperature