反应详情

温度

80 °C

To a flask containing 2,3-dichloronitrobenzene (387 mg, 2.01 mmol) was added 3 mL of piperidine, and the result was heated to 80° C. overnight. The reaction was diluted with EtOAc (30 mL), washed with water (2×30 mL), dried (Na2SO4) and concentrated in vacuo. Purification by preparative tlc (20% EtOAc-hexane) yielded 320 mg (66%) of the title compound as a yellow solid. 1H-NMR (CDCl3; 400 MHz): δ 7.56-7.50 (m, 2H), 7.04 (t, 1H, J=8.1 Hz), 3.04 (br s, 4H), 1.69 (br s, 4H), 1.59 (br s obscured by water, 2H).

1. washwashed with water (2×30 mL)
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated in vacuo
4. customPurification by preparative tlc (20% EtOAc-hexane)