反应详情

温度

70 °C

Tin (II) chloride (12.77 g, 67 mmol) was added to a solution of 1-benzyl-4-(2-nitrophenyl)piperazine (4.0 g, 13 mmol) in ethanol (50 mL) and the mixture was heated at 70° C. for 1 h. The solvent was evaporated under reduced pressure and the residue was diluted with ethyl acetate and washed with aqueous sodium hydroxide (2M, 4×). The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with EtOAc/Hexane (80:20 increasing to 75:25) to give the title compound as a pale yellow solid (2.61 g, 72%), δH (250 MHz, CDCl3) 7.38-7.25 (5H, m), 7.03-6.89 (2H, m), 6.77-6.70 (2H, m), 4.05-3.90 (2H, br s), 3.59 (2H, s), 2.96-2.92 (4H, m), and 2.65-2.55 (4H, br s).

1. customThe solvent was evaporated under reduced pressure
2. additionthe residue was diluted with ethyl acetate
3. washwashed with aqueous sodium hydroxide (2M, 4×)
4. dry with materialThe organic layer was dried (MgSO4)
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was purified by flash column chromatography on silica gel
7. washeluting with EtOAc/Hexane (80:20 increasing to 75:25)