تفاعل #155701

معادلة التفاعل

2-nitrophenanthrene

ethanol

hydrazine monohydrate

→

pale yellow solid

المردود 86.2%

2-aminophenanthrene

المردود 86.2%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder heating
2. 2
   درجة الحرارةreflux
3. 3
   استخلاصThen, the mixture was extracted with 2 L of toluene
4. 4
   أخرىAfter the water layer had been removed
5. 5
   تجفيفthe organic layer was dried with magnesium sulfate
6. 6
   أخرىAfter magnesium sulfate had been separated by filtration
7. 7
   أخرىthe solvent was removed by distillation under reduced pressure
8. 8
   أخرىThe residue was purified by silica gel column chromatography

الإجراء التجريبي

First, 134 g of 2-nitrophenanthrene, 1.00 g of palladium carbon, and 1.2 L of ethanol were loaded, and then 70 mL of hydrazine monohydrate were added to the mixture. The reaction solution was stirred for 4 hours under heating reflux. After having been cooled to room temperature, the reaction solution was poured into 3 L of water. Then, the mixture was extracted with 2 L of toluene. After the water layer had been removed, the organic layer was dried with magnesium sulfate. After magnesium sulfate had been separated by filtration, the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 100 g of a pale yellow solid were obtained (in 86% yield).

المصدر