反应详情

2-Bromo-5-nitroanisole (5.0 g, 21.5 mmol) and piperidine (8.5 ml) is stirred for 5 h at 105° C. under N2-atmosphere. Water (80 ml) is added and the mixture is extracted twice with CH2Cl2 (2×80 ml). The organic phases are washed with water and brine, dried (Na2SO4) and concentrated. The crude product is dissolved in AcOEt, SiO2 is then added and the solvent evaporate off In vacuo. The resulting powder is put on top of a chromatography column (SiO2; AcOEt/hexane 9:1) and the title compound eluted with hexane/AcOEt 9:1→4:1: MS: [M+1]+=237; Rf=0.2 (AcOEt/hexane 9:1).

1. extractionthe mixture is extracted twice with CH2Cl2 (2×80 ml)
2. washThe organic phases are washed with water and brine
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated
5. dissolutionThe crude product is dissolved in AcOEt
6. additionSiO2 is then added
7. customthe solvent evaporate off In vacuo
8. washthe title compound eluted with hexane/AcOEt 9:1→4:1