反应详情

To a stirred mixture of 1-(1-ethylpropyl)piperazine (175 μl, 1.0 mmol) and dry DCM (10 ml) was added 3-trifluoromethylphenyl chloroformate (250 mg, 1.1 mmol). The mixture was stirred overnight at room temperature and then diluted with DCM (50 ml). The reaction mixture was washed with 1 N NaOH (3×25 ml) and water (2×25 ml). The organic solution was concentrated and the residue was dissolved in a 0.5 N HCl solution (15 ml) and a small portion of acetonitrile. The acidic solution was concentrated and stirred with ethyl acetate (15 ml). The solid was isolated and dried to give 330 mg (86%) of the title compound as a solid. M.p. 260–261° C.

1. washThe reaction mixture was washed with 1 N NaOH (3×25 ml) and water (2×25 ml)
2. concentrationThe organic solution was concentrated
3. dissolutionthe residue was dissolved in a 0.5 N HCl solution (15 ml)
4. concentrationThe acidic solution was concentrated
5. stirringstirred with ethyl acetate (15 ml)
6. customThe solid was isolated
7. customdried