反应详情

To a solution of 1-(4-aminophenyl)piperidin-4-ol (3.7 g, 319 mmol) in 60 mL of HBr 48%, a solution of NaNO2 (1.38 g, 20 mmol) in 15 mL of water was slowly added at 0° C. The mixture was stirred for 30 minutes and added to a solution of CuBr (1.57 g, 11 mmol) in 50 mL of HBr 48%. The resulting mixture was stirred and refluxed for 2 hours. The suspension thus obtained was partitioned between 2N NaOH and ethyl acetate. The organic layer was washed with aqueous NaCl, dried over Na2SO4 and concentrated to afford crude compound as grey solid 4.6 g. MS (m/z): 256 (M)+

1. stirringThe resulting mixture was stirred
2. temperaturerefluxed for 2 hours
3. customThe suspension thus obtained
4. customwas partitioned between 2N NaOH and ethyl acetate
5. washThe organic layer was washed with aqueous NaCl
6. dry with materialdried over Na2SO4
7. concentrationconcentrated