反应详情

First, 100 g of 2-aminophenanthrene were dissolved in 750 mL of N,N-dimethyl sulfoxide, and then 83 g of 48% hydrobromic acid were dropped to the solution over 4 hours while the solution was stirred at room temperature. The mixture was continuously stirred at room temperature for 20 hours, and was then stirred at 100° C. for 1 hour under heat. After having been cooled to room temperature, the reaction solution was poured into 3 L of water. After the mixed solution had been neutralized with ammonia water, the crystal was obtained through separation by filtration. The resultant solid was recrystallized with ethanol and water. Thus, 126 g of a colorless crystal were obtained (in 90% yield).

1. stirringThe mixture was continuously stirred at room temperature for 20 hours
2. stirringwas then stirred at 100° C. for 1 hour
3. temperatureunder heat
4. temperatureAfter having been cooled to room temperature
5. customthe crystal was obtained through separation by filtration
6. customThe resultant solid was recrystallized with ethanol and water