反応 #155702

反応方程式

2-aminophenanthrene

hydrobromic acid

ammonia water

→

colorless crystal

収率 90.0%

2-amino-1-bromophenanthrene

収率 90.0%

溶媒

—

N,N-dimethyl sulfoxide

water

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture was continuously stirred at room temperature for 20 hours
2. 2
   workup.STIRRINGwas then stirred at 100° C. for 1 hour
3. 3
   温度under heat
4. 4
   温度After having been cooled to room temperature
5. 5
   その他the crystal was obtained through separation by filtration
6. 6
   その他The resultant solid was recrystallized with ethanol and water

実験手順

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).

出典