反应详情

To a solution of 2,2,2-trifluoro-1-piperazin-1-yl-ethanone (6 g, 32.94 mmol) and 1-benzhydrylazetidin-3-yl methanesulfonate (12.5 g, 39.38 mmol) in CH3CN (60 mL) was added DIPEA (12 mL, 68.89 mmol) at room temperature. The resulting mixture was refluxed for 2 h. The solvent was removed by evaporation and the residue was partitioned between CH2Cl2 and aq NaHCO3. The organic layer was washed with aq NaHCO3 (2×) and then extracted with 1N HCl (2×). The aqueous layer was cooled and then the pH adjusted with 1N NaOH until basic (pH=10). The resulting mixture was extracted with CH2Cl2 (2×). The organic layer was dried over MgSO4 and concentrated. The title compound was purified by reverse phase chromatography. MS m/z (M+H+) 404.2.

1. temperatureThe resulting mixture was refluxed for 2 h
2. customThe solvent was removed by evaporation
3. customthe residue was partitioned between CH2Cl2 and aq NaHCO3
4. washThe organic layer was washed with aq NaHCO3 (2×)
5. extractionextracted with 1N HCl (2×)
6. temperatureThe aqueous layer was cooled
7. extractionThe resulting mixture was extracted with CH2Cl2 (2×)
8. dry with materialThe organic layer was dried over MgSO4
9. concentrationconcentrated
10. customThe title compound was purified by reverse phase chromatography