反应详情

To a solution of 1-methoxy-4-methyl-2-(3,3,5,5-tetramethylcyclohexyl)benzene (1.0 g, 3.84 mmol) produced in Example (104b) in acetic acid (5 mL) was added 48% hydrobromic acid (10 mL, 59.3 mmol), followed by reflux for 12 hours. Saturated aqueous solution of sodium hydrogencarbonate was added to the cooled reaction mixture, and extraction was performed with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and the filtrate was concentrated under reduced pressure to give a residue, which was purified by silica gel column chromatography (ethyl acetate/heptane) to give 450 mg of the title compound as a light yellow oil.

1. temperatureby reflux for 12 hours
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. concentrationthe filtrate was concentrated under reduced pressure
4. customto give a residue, which
5. customwas purified by silica gel column chromatography (ethyl acetate/heptane)