反应详情

1-tert-Butoxycarbonyl-4-hydroxy-4-(2-quinolylmethyl)piperidine (5.95 g) was dissolved in anhydrous THF (50 ml), and methane sulfonylchloride (2.99 g) and triethylamine (7.3 ml) were added to the solution. The mixture was stirred at room temperature for two hours and concentrated under reduced pressure. Water and ethyl acetate were added to the mixture to thereby separate an organic phase, which was further washed with saturated brine, dried over sodium sulfate anhydrate, and concentrated under reduced pressure. The residue was dissolved in toluene (50 ml), and DBU (5.30 g) was added to the solution. The mixture was stirred at 60° C. for three hours and concentrated under reduced pressure. Water and ethyl acetate were added to the mixture to thereby separate an organic phase, which was further washed with saturated brine, dried over sodium sulfate anhydrate, and concentrated under reduced pressure. The resultant residue was subjected to silica gel column chromatography (developer: hexane-ethyl acetate (1:1)). The title compound was obtained through crystallization from hexane.

1. concentrationconcentrated under reduced pressure
2. additionWater and ethyl acetate were added to the mixture
3. customto thereby separate an organic phase, which
4. washwas further washed with saturated brine
5. dry with materialdried over sodium sulfate anhydrate
6. concentrationconcentrated under reduced pressure
7. dissolutionThe residue was dissolved in toluene (50 ml)
8. additionDBU (5.30 g) was added to the solution
9. stirringThe mixture was stirred at 60° C. for three hours
10. concentrationconcentrated under reduced pressure
11. additionWater and ethyl acetate were added to the mixture
12. customto thereby separate an organic phase, which
13. washwas further washed with saturated brine
14. dry with materialdried over sodium sulfate anhydrate
15. concentrationconcentrated under reduced pressure