反应详情

温度

10 °C

With stirring and cooling in a water bath (about 10° C.), a solution of NaNO2 (0.85 g; 12.3 mmol) in H2O (10 ml) was added dropwise over a period of 2.5 min to a solution of 21a (3.0 g; 12 mmol) in glacial acetic acid. After the addition had ended, the reaction mixture was stirred at room temperature for 0.5 h, H2O (60 ml) was added and stirring at room temperature was continued for 3 h. The light-beige precipitate was filtered off, washed with water and dried under reduced pressure over CaCl2.

1. additionAfter the addition
2. stirringthe reaction mixture was stirred at room temperature for 0.5 h
3. stirringstirring at room temperature
4. filtrationThe light-beige precipitate was filtered off
5. washwashed with water
6. dry with materialdried under reduced pressure over CaCl2