반응 #674290

반응 방정식

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

Water

Na2CO3

→

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

수율 96.0%

용매

EtOH AcOH

반응 조건

후처리

1. 1
   온도The mixture was then refluxed for 75 min
2. 2
   여과The precipitate was collected by filtration
3. 3
   농축The filtrate was concentrated by evaporator and in vacuo
4. 4
   기타to give black residue
5. 5
   추출extracted with ether (3×200 mL)
6. 6
   세척The combined ethereal solution was washed with saturated NaHCO3 (2×60 mL), H2O (60 mL) and brine (60 mL)
7. 7
   건조dried over anhydrous Na2SO4
8. 8
   농축concentrated by evaporator in vacuo

실험 절차

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.

출처