反应详情

A solution of Compound 68 (0.8 g, 2.43 mmol) in dichloromethane was added slowly to a stirred solution of piperazine (628 mg g, 7.29 mmol) in dichloromethane at room temperature. The solution was stirred overnight at room temperature. The solvent was then removed under reduced pressure. The residue was taken in water, sonicated briefly, and filtered. The solids were dissolved in ethyl acetate and washed by water. The organic layer was dried over Na2SO4 and concentrated to yield 0.9 g (98%) of yellow solids. M.P. 156° C. 1H NMR (DMSO-d6): δ 2.94 (m, 4H), 3.55 (m, 4H), 5.47 (s, 2H), 7.19 (m, 2H), 7.24 (m, 1H), 7.31 (m, 2H), 7.39 (d, J=8.9 Hz, 1H), 7.64 (dd, J=2.6, 8.9 Hz, 1H), 7.81 (d, J=2.6 Hz, 1H). EIMS m/z 379 (M+1).

1. customThe solvent was then removed under reduced pressure
2. customsonicated briefly
3. filtrationfiltered
4. dissolutionThe solids were dissolved in ethyl acetate
5. washwashed by water
6. dry with materialThe organic layer was dried over Na2SO4
7. concentrationconcentrated