반응 #41533

반응 방정식

ammonium chloride

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

→

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

용매

methanol

water

반응 조건

후처리

1. 1
   기타the reaction liquid
2. 2
   온도was heated
3. 3
   온도under reflux for 3 hours
4. 4
   기타The reaction liquid
5. 5
   여과was filtered
6. 6
   기타the solvent was evaporated away under reduced pressure
7. 7
   workup.ADDITIONThe residue was diluted with ethyl acetate
8. 8
   세척washed with water
9. 9
   건조dried with anhydrous magnesium sulfate
10. 10
    기타The solvent was evaporated away under reduced pressure
11. 11
    기타the resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)
12. 12
    기타to obtain the entitled compound as a pale yellow oily substance

실험 절차

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.

출처