反应详情

A solution of Compound 8 (15 g, 48 mmol) in dichloromethane was added slowly to a stirred solution of piperazine (12 g, 144 mmol) in dichloromethane at room temperature. The solution was stirred overnight at room temperature. The solvent was removed under reduced pressure. The residue was taken in water, sonicated briefly, and filtered. The solid was dissolved in ethyl acetate and washed by water. The organic layer was dried over Na2SO4 and concentrated to yield 17.17 g (98%) of yellow solids. 1H NMR (DMSO-d6): δ 2.8 (m, 2H), 3.0 (m, 2H), 3.6 (m, 2H), 3.7 (m, 2H), 5.45 (s, 2H), 7.1 (m, 2H), 7.3 (m, 3H), 7.4 (m, 1H), 7.6 (m, 1H), 7.90 (t, J=8.2 Hz, 1H); EIMS: 363 (M+H).

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