反応 #41569

反応方程式

potassium nitrate

trifluoroacetic acid

tert-butyl (3-fluoro-4-(6-methanesulfonyl-pyridin-3-yloxy)-phenyl)-carbamate

→

5-fluoro-4-(6-methanesulfonyl-pyridin-3-yloxy)-2-nitro-phenylamine

反応条件

後処理

1. 1
   その他obtained in (step 2)
2. 2
   その他the reaction liquid
3. 3
   その他the solvent was evaporated away under reduced pressure
4. 4
   workup.ADDITIONThe residue was diluted with ethyl acetate
5. 5
   洗浄washed with aqueous saturated sodium bicarbonate and saturated saline in order
6. 6
   乾燥dried with anhydrous sodium sulfate
7. 7
   その他The solvent was evaporated away under reduced pressure
8. 8
   その他the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/2)
9. 9
   その他to obtain the entitled compound

実験手順

0.98 g of potassium nitrate was added to a trifluoroacetic acid (35 ml) solution of 3.38 g of tert-butyl (3-fluoro-4-(6-methanesulfonyl-pyridin-3-yloxy)-phenyl)-carbamate obtained in (step 2), the reaction liquid was stirred at room temperature for 1 hour, 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 sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/2) to obtain the entitled compound.

出典