反应详情

To 1-(5-chloro-2-nitro-phenyl)-piperidine (197 mg, 0.810 mmol, as prepared in Example 3, step (a)) in 1.5 mL of DMF was added 4 mL of 0.5 M NaOEt in EtOH (1.94 mmol). The resultant solution was heated at 90° C. for 24 h. The reaction was diluted with EtOAc (50 mL) and washed with water (50 mL), dried (Na2SO4) and concentrated in vacuo. Purification by preparative tic (20% EtOAc-hexane) gave 110 mg (54%) of the title compound. Mass spectrum (ESI, m/z): Calcd. for C13H18N2O3, 251.1 (M+H), found 251.1.

1. washwashed with water (50 mL)
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated in vacuo
4. customPurification by preparative tic (20% EtOAc-hexane)