反应详情

To a solution of 2-piperazin-1-yl-pyrimidine (2.48 g, 15.10 mmol, Alfa) and methanesulfonic acid 1-benzhydryl-azetidin-3-yl ester (4 g, 12.6 mmol, Oakwood) in CH3CN (40 mL) was added DIPEA (2.63 mL, 15.10 mmol) at room temperature. The resulting mixture was then refluxed for 2 h. The solvent was removed by evaporation and the residue was partitioned between CH2Cl2 and aqueous NaHCO3. The organic layer was washed with aqueous NaHCO3 (2×) and then extracted with 1N HCl (2×). The aqueous layer was cooled and then pH adjusted with 1N NaOH. The resulting mixture was extracted with CH2Cl2 (2×). The organic layer was dried over MgSO4 and concentrated. The resulting residue was purified by MPLC to yield 2-[4-(1-benzhydryl-azetidin-3-yl)-piperazin-1-yl]-pyrimidine.

1. temperatureThe resulting mixture was then refluxed for 2 h
2. customThe solvent was removed by evaporation
3. customthe residue was partitioned between CH2Cl2 and aqueous NaHCO3
4. washThe organic layer was washed with aqueous 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 resulting residue was purified by MPLC