反应详情

To a solution of 2-[1-[2-[4-(p-toluidino)piperidin-1-yl]ethyl]cyclobutyl]ethanol (synthesized in Example 66) (175 mg) in tetrahydrofuran (3 mL) was added triethylamine (0.46 mL) and 2-furoyl chloride (0.16 mL) sucessively. The solution was stirred at room temperature for 40 minutes. To the reaction solution were added methanol (4 mL) and a 3N aqueous potassium hydroxide solution (2 mL). The solution was stirred for additional 30 minutes. Saturated sodium chloride solution was added to the reaction solution and it was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by chromatography [NH silica gel, hexane-ethyl acetate (1:1)] to give the title compound (159 mg).

1. stirringThe solution was stirred for additional 30 minutes
2. extractionwas extracted with ethyl acetate
3. washThe organic layer was washed with saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by chromatography [NH silica gel, hexane-ethyl acetate (1:1)]