反应详情

温度

80 °C

4-Chloro-2,5-dimethoxynitrobenzene (5.0 g, 23 mmol) was dissolved in DMSO (50 mL). K2CO3 (4.8 g, 34 mmol) and 4-piperidinopiperidine (3.9 g, 23 mmol) were added and the reaction mixture was heated to 80° C. and allowed to stir over the weekend. The mixture was then poured into H2O and extracted with EtOAc (2×). The combined organics were dried with MgSO4, filtered, and concentrated in vacuo. The resulting residue was adsorbed onto silica gel and flash chromatographed to give the title compound of step A (3.0 g, 37%). MS (M+H, ES+) 350.

1. extractionextracted with EtOAc (2×)
2. dry with materialThe combined organics were dried with MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customchromatographed