反应详情

A flask containing H2SO4 (12 mL, 219 mmol) and P2O5 (12 g, 88 mmol) was cooled in an ice-water bath for 20 minutes. To this viscous mixture was slowly added diethyl 2-(2-(2-fluorophenyl)-2-methylpropanoyl)malonate (7.1 g, 22 mmol). The ice bath was removed, and the mixture was stirred at room temperature for 1 hour before being poured over crushed ice and diluted with IPAc (100 mL). Water (50 mL) was added, and the resulting mixture was extracted with EtOAc (2×100 mL). The organic layers were combined, dried over Na2SO4, filtered, and concentrated in vacuo to afford a yellow oil that was further purified using flash chromatography (10% EtOAc/hexane, 2.5 g). MS (m/z)=279 (M+H)+.

1. temperaturewas cooled in an ice-water bath for 20 minutes
2. customThe ice bath was removed
3. additionbefore being poured
4. customover crushed ice
5. additiondiluted with IPAc (100 mL)
6. additionWater (50 mL) was added
7. extractionthe resulting mixture was extracted with EtOAc (2×100 mL)
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customto afford a yellow oil that
12. customwas further purified