反应详情

To a solution of 1.49 g (3.48 mM) of N-(3-phenylpropan-1-yl)-N-[1-tert-butoxycarbonylpiperidin-4-ylmethyl]trifluoroacetamide in ethanol (10 ml) was added 1.0 ml (12 mM) of 12N-hydrochloric acid at room temperature and the mixture was stirred for 20 hours. The solvent was then distilled off under reduced pressure and 3 ml (36 mM) of 12N-hydrochloric acid was added to the residue. This mixture was stirred at room temperature for 20 minutes. To this reaction mixture was added ethanol and the solvent was distilled off under reduced pressure to provide 1.29 g (quantitative) of a crude product as white solid. To a solution of 0.33 g (0.90 mM) of this crude product in ethanol (4 ml) was added 4 ml (4 mM) of 1N-aqueous solution of sodium hydroxide at room temperature and the mixture was stirred for 30 minutes. The ethanol was then distilled off under reduced pressure and the residue was extracted with chloroform. The organic layer was washed with saturated aqueous solution of sodium chloride and dried over MgSO4. The solvent was then distilled off under reduced pressure to provide the title compound.

1. distillationThe solvent was then distilled off under reduced pressure and 3 ml (36 mM) of 12N-hydrochloric acid
2. additionwas added to the residue
3. stirringThis mixture was stirred at room temperature for 20 minutes
4. additionTo this reaction mixture was added ethanol
5. distillationthe solvent was distilled off under reduced pressure
6. customto provide 1.29 g (quantitative) of a crude product as white solid
7. stirringthe mixture was stirred for 30 minutes
8. distillationThe ethanol was then distilled off under reduced pressure
9. extractionthe residue was extracted with chloroform
10. washThe organic layer was washed with saturated aqueous solution of sodium chloride
11. dry with materialdried over MgSO4
12. distillationThe solvent was then distilled off under reduced pressure