Reaktion #46820

Reaktionsgleichung

2-(2-Methoxy-ethoxy)-6-nitro-phenylamine

NaOH

→

3-(2-Methoxy-ethoxy)-benzene-1,2-diamine

Lösungsmittel

ethyl acetate

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction mixture was heated
2. 2
   Temperaturto reflux for 6 h
3. 3
   workup.ADDITIONwere added
4. 4
   Filtrationthe inorganic precipitate was filtered
5. 5
   Waschenwashed extensivley with ethyl acetate
6. 6
   ExtraktionThe filtrate was extracted with exthyl acetate (3×100 ml)
7. 7
   Trocknenthe combined organic layers were dried over MgSO4
8. 8
   Sonstigethe solvents were removed under reduced pressure
9. 9
   SonstigeThe remaining product was pure enough for the next reaction step

Vorschrift

To a solution of 1 g 2-(2-Methoxy-ethoxy)-6-nitro-phenylamine in 10 mL ethyl acetate and 3 mL ethanol, 4.4 g SnCl2 dihydrate were added and the reaction mixture was heated to reflux for 6 h. Then, after cooling 50 mL 2 M NaOH were added and the inorganic precipitate was filtered and washed extensivley with ethyl acetate. The filtrate was extracted with exthyl acetate (3×100 ml), the combined organic layers were dried over MgSO4, and the solvents were removed under reduced pressure. The remaining product was pure enough for the next reaction step.

Quelle