反应详情

温度

20 °C

A solution of 5.0 g (0.025 mole) of 2'-amino-2-(methylsulfinyl)-acetophenone, 30 ml (0.03 mole) of cold (15°C) 1N hydrochloric acid and 100 ml of cold water cooled to 5°C. A solution of 2.07 g (0.03 mole) of sodium nitrite in 10 ml of water was added over a period of 3 minutes with stirring, keeping the temperature at 5°C. A deep red color developed as yellow solid separated. The mixture was allowed to warm up to 20°C. After 15 minutes at 20° the product was filtered, washed with water, 2-propanol and then ether. Wt 5.0 g (64%) mp. 266°-269°. Recrystallization from N,N-dimethylformamide gave pure, white crystals melting at 274°-276°C.

1. customat 5°C
2. customseparated
3. filtrationAfter 15 minutes at 20° the product was filtered
4. washwashed with water, 2-propanol
5. customRecrystallization from N,N-dimethylformamide
6. customgave pure