反应详情

温度

0 °C

0.22 g (1 mmol) 2-cyano-4-methoxy-5-n-butoxyphenylamine and 3 mL (10 mol/L) hydrochloric acid were added into a round bottom flask. The solution was cooled to 0° C. and diazotized with sodium nitrite (0.072 g, 1 mmol) dissolved in water (1.0 mL), which was added dropwise to the solution. The mixture was stirred to react for 20 min. After adjusting the pH to 5˜6 with sodium acetate, the ethanol solution of aniline (0.093 g, 1 mmol) was added dropwise to the reaction mixture to react for 2 h under stirring, while maintaining the reaction temperature at between 0˜5° C., and using sodium acetate to keep the pH value at 5-6. The solution was kept overnight, filtered, and washed with water till colorless. The crude product was purified on a silica gel column with petroleum ether:ethyl acetate (v/v)=15:1 to yield 0.154 g of orange-yellow solid crystal product with a recovery rate of 47.5%.

1. additionwhich was added dropwise to the solution
2. customto react for 20 min
3. customto react for 2 h
4. stirringunder stirring
5. temperaturewhile maintaining the reaction temperature at between 0˜5° C.
6. filtrationfiltered
7. washwashed with water till colorless
8. customThe crude product was purified on a silica gel column with petroleum ether