反応 #41534

反応方程式

potassium nitrate

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

→

compound

3-chloro-2,4-bis(pyridin-3-yloxy)-6-nitroaniline

溶媒

trifluoroacetic acid

反応条件

後処理

1. 1
   その他the reaction liquid
2. 2
   その他the solvent was evaporated away under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with ethyl acetate
4. 4
   洗浄washed with aqueous saturated sodium bicarbonate and saturated saline in order
5. 5
   乾燥dried with anhydrous magnesium sulfate
6. 6
   その他The solvent was evaporated away under reduced pressure
7. 7
   その他the resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)

実験手順

315 mg of potassium nitrate was added to a trifluoroacetic acid (20 ml) solution of 891 mg of 3-chloro-2,4-bis(pyridin-3-yloxy)aniline, and the reaction liquid was stirred overnight at room temperature, and then the solvent was evaporated away under reduced pressure. The residue was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate and saturated saline in order, 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 an orange solid.

出典