反应详情

温度

100 °C

The crude diketone from step 1 (about 1.05 mmol) was treated with acetic acid (5 mL) and 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 Na2CO3 in CH2Cl2, dried over MgSO4, then filtered through a pad of silica gel and the product washed off with EtOAc. The filtrate and washings were concentrated under vacuum. The crude product was purified by preparative layer chromatography on a 0.05×20×20 cm silica gel GF plate, developing with 30% EtOAc in hexanes, to afford 7-amino-9a-butyl-4-ethyl-6,8-difluoro-1,2,9,9a-tetrahydro-3H-fluoren-3-one (0.16 g, 48%) as a yellow solid.

1. temperatureAfter cooling to room temperature
2. dry with materialdried over MgSO4
3. filtrationfiltered through a pad of silica gel
4. washthe product washed off with EtOAc
5. concentrationThe filtrate and washings were concentrated under vacuum
6. customThe crude product was purified by preparative layer chromatography on a 0.05×20×20 cm silica gel GF plate