反应详情

温度

75 °C

10.7 g of 4-toluidine was added dropwise to 27% aqueous sulfuric acid solution which contains 5.4 g of sulfuric acid. After the reaction mixture was heated to 75° C., 8.4 g of ammonium thiocyanate in a solid state was slowly added thereto. Upon complete addition, the reaction mixture was stirred for 20 hours at 80° C. to 90° C. After adding toluene, the whole mixture was refluxed for one hour, cooled to room temperature and then adjusted to pH 7.5 to 8 by slowly adding ammonia water. The resulting white solid was filtered, washed once with each of water and toluene and then dried under reduced pressure to obtain the title compound as a white solid (Yield: 78.5%).

1. additionUpon complete addition
2. temperaturethe whole mixture was refluxed for one hour
3. temperaturecooled to room temperature
4. filtrationThe resulting white solid was filtered
5. washwashed once with each of water and toluene
6. customdried under reduced pressure