تفاعل #155713

معادلة التفاعل

2-aminophenanthrene

hydrobromic acid

ammonia water

→

colorless crystal

المردود 90.0%

2-amino-1-bromophenanthrene

المردود 90.0%

المذيبات

—

N,N-dimethyl sulfoxide

water

ظروف التفاعل

المعالجة

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
   درجة الحرارةunder heat
4. 4
   درجة الحرارةAfter having been cooled to room temperature
5. 5
   أخرىthe crystal was separated by filtration
6. 6
   أخرىThe resultant solid was recrystallized with ethanol and water

الإجراء التجريبي

First, 10.0 g of 2-aminophenanthrene were dissolved in 75 mL of N,N-dimethyl sulfoxide, and then 8.3 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 300 mL of water. After the mixed solution had been neutralized with ammonia water, the crystal was separated by filtration. The resultant solid was recrystallized with ethanol and water. Thus, 12.6 g of a colorless crystal were obtained (in 90% yield).

المصدر