反应详情

A mixture of 2-(4-hydrazinophenyl)ethanol hydrochloride (J. Med. Chem., 1999, 42, 2504, 202 mg, 1.07 mmol) and benzoyl-1,1,1-trifluoroacetone (278 mg, 1.28 mmol) in ethanol (13 mL) was heated under reflux overnight. After removal of the solvent, the resulting residue was partitioned between dichloromethane and water. Organic phase was washed with brine and dried (Na2SO4). After removal of the solvent, the crude product was purified by TLC with hexane/ethyl acetate (1:1) to afford 200 mg (56%) of the title compound as yellow solids: MS (ESI) m/z 333 [M+H]+, 1H-NMR (CDCl3) δ 7.36-7.20 (9H, m), 6.74 (1H, s), 3.86 (2H, br.s), 2.89 (2H, t, J=6.6 Hz).

1. temperaturewas heated
2. temperatureunder reflux overnight
3. customAfter removal of the solvent
4. customthe resulting residue was partitioned between dichloromethane and water
5. washOrganic phase was washed with brine
6. dry with materialdried (Na2SO4)
7. customAfter removal of the solvent
8. customthe crude product was purified by TLC with hexane/ethyl acetate (1:1)