反应详情

温度

90 °C

Compound 245d (10.46 g, 45.74 mmol) was added portionwise to BF3.Et2O at 40° C. The mixture was then heated at 90° C. for 3 hrs. After cooling down to room temperature, the reaction mixture was poured into crushed ice and extracted with EtOAc. Organics were dried over Na2SO4, filtered, concentrated under reduced pressure, and purified by chromatography on silica gel (petroleum ether/EtOAc). The compound obtained was recrystallized from EtOH to yield compound 246d as a brown solid in 63% yield. 1H NMR (DMSO-d6, 400 MHz) δ (ppm) 3.96 (s, 3H), 6.79 (d, J=9.10 Hz, 1H), 7.52 (d, J=9.10 Hz, 1H), 11.40 (s, 1H).

1. temperatureAfter cooling down to room temperature
2. additionthe reaction mixture was poured
3. custominto crushed ice
4. extractionextracted with EtOAc
5. dry with materialOrganics were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. custompurified by chromatography on silica gel (petroleum ether/EtOAc)
9. customThe compound obtained
10. customwas recrystallized from EtOH