反应详情

温度

100 °C

The diketone from step 1 (0.51 g, 1.73 mmol) was treated with acetic acid (5 mL,) and aqueous 6N HCl (5 mL). The resulting solution was stirred and heated in an oil bath at 100° C. for 1.5 hours. After cooling to room temperature, the mixture was poured into a slurry of solid NaHCO3 in CH2Cl2, then filtered through a pad of silica gel and the product was washed off with EtOAc. The filtrate and washings were concentrated under vacuum. The residue was purified by flash chromatography on a Biotage 40M KP-Sil column, eluting with 4:1 to 3:1 hexanes-EtOAc. The product containing fractions were evaporated under vacuum to provide 7-amino-9a-butyl-6-fluoro-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (0.40 g, 83%) as a yellow solid

1. temperatureAfter cooling to room temperature
2. filtrationfiltered through a pad of silica gel
3. washthe product was washed off with EtOAc
4. concentrationThe filtrate and washings were concentrated under vacuum
5. customThe residue was purified by flash chromatography on a Biotage 40M KP-Sil column
6. washeluting with 4:1 to 3:1 hexanes-EtOAc
7. additionThe product containing fractions
8. customwere evaporated under vacuum