反应详情

温度

138 °C

A mixture of 350 mg (1.45 mmol) of 1-(5-chloro-2-nitro-phenyl)-piperidine (as prepared in Example 4, step (a)) and 482 μL (4.35 mmol) of 1-methylpiperazine was heated in a sealed vial at 138° C. for 30 h. The mixture was cooled and poured into 60 mL of water and extracted with EtOAc (2×20 mL). The combined extracts were washed with brine (30 mL), dried (Na2SO4) and concentrated in vacuo to afford 436 mg (99%) of the title compound as a yellow resin: Mass spectrum (ESI, m/z): Calcd. for C16H24N4O2, 305.2 (M+H), found 305.2.

1. temperatureThe mixture was cooled
2. extractionextracted with EtOAc (2×20 mL)
3. washThe combined extracts were washed with brine (30 mL)
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo