反应详情

温度

100 °C

A solution of the crude diketone from step 1 in acetic acid (1 mL) and 6N HCl (1 mL) was stirred and heated in an oil bath at 100° C. for 5 hours. After cooling, the reaction mixture was diluted with EtOAc (20 mL), washed with water (10 mL) and brine (10 mL), dried over MgSO4, filtered, and the solvent evaporated under vacuum. The residue was purified by preparative layer chromatography on two 0.1×20×20 cm silica gel GF plates, using 5% EtOAc in CH2Cl2 as developing solvent, to afford 9a butyl-4,8-dimethyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (84 mg) as a gum.

1. temperatureAfter cooling
2. washwashed with water (10 mL) and brine (10 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customthe solvent evaporated under vacuum
6. customThe residue was purified by preparative layer chromatography on two 0.1×20×20 cm silica gel GF plates