反应详情

温度

80 °C

Into a 50-mL round-bottom flask were placed N,N-dimethylformamide (2.15 g, 29.45 mmol) and phosphoryl trichloride (20.3 g, 132.7 mmol) and the mixture was cooled to 0° C. Then, N-(4-bromophenyl)-2-phenylacetamide (5.7 g, 17.87 mmol, Intermediate 23: step a) was added in portions. The resulting solution was heated at 80° C. for 5 hours, then concentrated under vacuum, followed by dilution with 50 mL of H2O, and then extraction with 3×50 mL of ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was purified by FCC (1:10 EtOAc/petroleum ether) to afford the title compound as a yellow solid.

1. customInto a 50-mL round-bottom flask were placed
2. concentrationconcentrated under vacuum
3. extractionextraction with 3×50 mL of ethyl acetate
4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by FCC (1:10 EtOAc/petroleum ether)