反应详情

温度

80 °C

A solution of 1-[3-(3-fluoro-piperidin-1-yl)-4-nitro-phenyl]4-methyl-piperazine (as prepared in the previous step, 60 mg, 0.19 mmol) in 2:1 EtOH:water (6 mL), was treated with glacial AcOH (1 drop) and iron powder (10 mg, 0.93 mmol). The mixture was heated to 80° C. for 30 min. The reaction cooled to room temperature, diluted with EtOAc and washed with saturated aqueous NaHCO3. The aqueous layer was extracted with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to afford the title compound (46 mg, 84%), which was used directly in the next reaction. LC-MS (ESI, m/z): Calcd. for C16H25FN4 293.2 (M+H), found 293.2.

1. temperatureThe reaction cooled to room temperature
2. washwashed with saturated aqueous NaHCO3
3. extractionThe aqueous layer was extracted with EtOAc
4. dry with materialThe combined organic layers were dried over MgSO4
5. concentrationconcentrated in vacuo