反应详情

温度

150 °C

To title compound 477 (3.12 g, 15.14 mmol) was added PPA (15 mL). The mixture was heated to 150° C. for 1 h then poured over water. The aqueous was basified with conc. NH4OH (exotherm) at 0° C. Water was added until everything was dissolved. The mixture was extracted with ethyl acetate (×4). The organics were washed with brine, died over Na2SO4, filtered and concentrated to a brown paste. The residue was purified by flash chromatography (0% to 70% ethyl acetate in hexanes) to afford title compound 478 (0.9 g, 32%) as a brown solid. MS (m/z): 189.1 (M+H).

1. dissolutionwas dissolved
2. extractionThe mixture was extracted with ethyl acetate (×4)
3. washThe organics were washed with brine
4. filtrationfiltered
5. concentrationconcentrated to a brown paste
6. customThe residue was purified by flash chromatography (0% to 70% ethyl acetate in hexanes)