تفاعل #674290

معادلة التفاعل

3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine

Water

Na2CO3

→

3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine

المردود 96.0%

المذيبات

EtOH AcOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was then refluxed for 75 min
2. 2
   ترشيحThe precipitate was collected by filtration
3. 3
   تركيزThe filtrate was concentrated by evaporator and in vacuo
4. 4
   أخرىto give black residue
5. 5
   استخلاصextracted with ether (3×200 mL)
6. 6
   غسيلThe combined ethereal solution was washed with saturated NaHCO3 (2×60 mL), H2O (60 mL) and brine (60 mL)
7. 7
   تجفيفdried over anhydrous Na2SO4
8. 8
   تركيزconcentrated by evaporator in vacuo

الإجراء التجريبي

To a suspension of 3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine (10 g, 30 mmol) in EtOH/AcOH (200/250 mL) was added iron powder (16.75 g, 300 mmol) in one portion. The mixture was then refluxed for 75 min. The reaction mixture was allowed to cool to room temperature. The precipitate was collected by filtration. The filtrate was concentrated by evaporator and in vacuo to give black residue. The black residue was combined with the collected solid. Water (300 mL) was added and the aqueous mixture was neutralized with Na2CO3, then extracted with ether (3×200 mL). The combined ethereal solution was washed with saturated NaHCO3 (2×60 mL), H2O (60 mL) and brine (60 mL), dried over anhydrous Na2SO4, concentrated by evaporator in vacuo to afford 3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine (8.67 g, 96%) as an off-white solid.

المصدر