反应详情

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.

1. customthe reaction liquid
2. temperaturewas heated
3. temperatureunder reflux for 3 hours
4. customThe reaction liquid
5. filtrationwas filtered
6. customthe solvent was evaporated away under reduced pressure
7. additionThe residue was diluted with ethyl acetate
8. washwashed with water
9. dry with materialdried with anhydrous magnesium sulfate
10. customThe solvent was evaporated away under reduced pressure
11. customthe resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)
12. customto obtain the entitled compound as a pale yellow oily substance