تفاعل #41533

معادلة التفاعل

ammonium chloride

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

→

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

المذيبات

methanol

water

ظروف التفاعل

المعالجة

1. 1
   أخرىthe reaction liquid
2. 2
   درجة الحرارةwas heated
3. 3
   درجة الحرارةunder reflux for 3 hours
4. 4
   أخرىThe reaction liquid
5. 5
   ترشيحwas filtered
6. 6
   أخرىthe solvent was evaporated away under reduced pressure
7. 7
   workup.ADDITIONThe residue was diluted with ethyl acetate
8. 8
   غسيلwashed with water
9. 9
   تجفيفdried with anhydrous magnesium sulfate
10. 10
    أخرىThe solvent was evaporated away under reduced pressure
11. 11
    أخرىthe resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)
12. 12
    أخرىto obtain the entitled compound as a pale yellow oily substance

الإجراء التجريبي

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.

المصدر