反应 #41533

反应方程式

ammonium chloride

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

→

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

溶剂

methanol

water

反应条件

后处理

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

实验过程

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.

来源