反应详情

温度

85 °C

A solution of (2SR,9aRS)-9a-butyl-2,4-dimethyl-7-methoxymethoxy-2-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (40 mg, 0.11 mmol) in methanol (approx. 0.5-1 mL) was placed under a nitrogen atmosphere and treated with 2N aqueous HCl (0.165 mL, 0.37 mmol). The resulting yellow solution was stirred and heated in an oil bath at 85° C. for 60 minutes. On cooling, the mixture deposited white crystals. The mixture was cooled in an ice bath and filtered. The crystalline product was washed with ice-cold 5:1 MeOH-2N HCl (2×2 mL) and dried under vacuum to afford (2SR,9aRS)-9a-butyl-2,4-dimethyl-7-hydroxy-2-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.

1. temperatureOn cooling
2. temperatureThe mixture was cooled in an ice bath
3. filtrationfiltered
4. washThe crystalline product was washed with ice-cold 5:1 MeOH-2N HCl (2×2 mL)
5. customdried under vacuum