反应详情

温度

0 °C

To a solution of N2-methyl-N2-(tetrahydro-2H-pyran-4-yl)pyridine-2,5-diamine (150 mg, 0.73 mmol) in 2 mL of aq HBr was added a solution of NaNO2 (55 mg, 0.80 mmol) in 1 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 (220 mg, 1.53 mmol) in 2 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, purified on TLC (EA:PE=1:1) to give white solid. MS (m/z): 273 (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. custompurified on TLC (EA:PE=1:1)
9. customto give white solid