反应详情

温度

60 °C

To a solution of 4-(2-methylmorpholino)aniline (7.21 g, 37.5 mmol) in 100 mL HBr in water (40%), a solution of NaNO2 (2.59 g, 37.5 mmol) in 15 mL water was added slowly at −10° C.˜0° C. The mixture was stirred for 30 minutes and was added dropwise to a solution of CuBr (2.96 g, 20.6 mmol) in 30 mL HBr in water (40%). The resulting mixture was stirred and heated at 60° C. for 2 hours. Then the reaction solution was adjusted by 2N NaOH solution to pH>7. Extracted by EA, the combined organic phase was washed with brine, dried and concentrated to give crude product as black oil. MS (m/z): 256 (M+H)+; 258 (M+3)+.

1. stirringThe resulting mixture was stirred
2. extractionExtracted by EA
3. washthe combined organic phase was washed with brine
4. customdried
5. concentrationconcentrated
6. customto give crude product as black oil