反应详情

A solution of 1.2 g of trans-4-(4'-decyl-4-biphenylyl)cyclohexyl tetrahydropyranyl ether in 40 ml of methanol and 2 ml of diethyl ether was treated with a solution of 7.3 mg of bistrimethylsilyl sulfate in 2 ml of dichloromethane. The reaction mixture was stirred at room temperature for 2 hours and then treated with 0.2 ml of pyridine. Subsequently, the reaction mixture was concentrated and the residue was then taken up in 50 ml of dichloromethane, washed twice with water, dried over magnesium sulfate, filtered and again concentrated. The residue was purified by chromatography on silica gel with toluene/ethyl acetate (vol. 9;1). Recrystallization from methanol gave 0.5 g of trans-4-(4'-decyl-4-biphenylyl)cyclohexanol.

1. concentrationSubsequently, the reaction mixture was concentrated
2. washwashed twice with water
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationagain concentrated
6. customThe residue was purified by chromatography on silica gel with toluene/ethyl acetate (vol. 9;1)
7. customRecrystallization from methanol