反应详情

温度

0 °C

To a solution of N-(1-(4-aminophenyl)piperidin-4-yl)-N-methylacetamide (479.7 mg, 1.94 mmol) in 6 mL of aq HBr was added a solution of NaNO2 (147 mg, 2.13 mmol) in 2 mL of H2O at 0° C., then the mixture was stirred at 0° C. for 40 minutes. After that, the mixture was poured into a solution of CuBr (584 mg, 4.07 mmol) in 6 mL aq HBr at 0° C., the reaction was heated to 60° C. and stirred for 2 hours. After cooling, the mixture was based with 2M NaOH to pH=8-9 and extracted with EA, washed with H2O and brine, dried and concentrated to give black solid. MS (m/z): 313 (M+H)+

1. temperaturethe reaction was heated to 60° C.
2. stirringstirred for 2 hours
3. temperatureAfter cooling
4. extractionextracted with EA
5. washwashed with H2O and brine
6. customdried
7. concentrationconcentrated
8. customto give black solid