反応 #41533

反応方程式

ammonium chloride

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

→

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

溶媒

methanol

water

反応条件

後処理

1. 1
   その他the reaction liquid
2. 2
   温度was heated
3. 3
   温度under reflux for 3 hours
4. 4
   その他The reaction liquid
5. 5
   ろ過was filtered
6. 6
   その他the solvent was evaporated away under reduced pressure
7. 7
   workup.ADDITIONThe residue was diluted with ethyl acetate
8. 8
   洗浄washed with water
9. 9
   乾燥dried with anhydrous magnesium sulfate
10. 10
    その他The solvent was evaporated away under reduced pressure
11. 11
    その他the resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)
12. 12
    その他to obtain the entitled compound as a pale yellow oily substance

実験手順

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.

出典