Reaktion #41533

Reaktionsgleichung

ammonium chloride

3-chloro-2,4-bis(pyridin-3-yloxy)-nitrobenzene

→

3-chloro-2,4-bis(pyridin-3-yloxy)aniline

Lösungsmittel

methanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reaction liquid
2. 2
   Temperaturwas heated
3. 3
   Temperaturunder reflux for 3 hours
4. 4
   SonstigeThe reaction liquid
5. 5
   Filtrationwas filtered
6. 6
   Sonstigethe solvent was evaporated away under reduced pressure
7. 7
   workup.ADDITIONThe residue was diluted with ethyl acetate
8. 8
   Waschenwashed with water
9. 9
   Trocknendried with anhydrous magnesium sulfate
10. 10
    SonstigeThe solvent was evaporated away under reduced pressure
11. 11
    Sonstigethe resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)
12. 12
    Sonstigeto obtain the entitled compound as a pale yellow oily substance

Vorschrift

963 mg of ammonium chloride and 503 mg of iron powder were added to a suspension of 1.2 g of 3-chloro-2,4-bis(pyridin-3-yloxy)-nitrobenzene in 15 ml of methanol and 7.5 ml of water, and the reaction liquid was heated under reflux for 3 hours. The reaction liquid was filtered, and the solvent was evaporated away under reduced pressure. The residue was diluted with ethyl acetate, washed with water, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate) to obtain the entitled compound as a pale yellow oily substance.

Quelle