反応 #41553

反応方程式

sodium bicarbonate

potassium nitrate

trifluoroacetic acid

1-(2-(5-amino-2-(4-methanesulfonyl-phenoxy)-phenyl)-pyrrolidin-1-yl)-2,2,2-trifluoro-ethanone

→

compound

1-(2-(5-amino-2-(4-methanesulfonyl-phenoxy)-4-nitro-phenyl)-pyrrolidin-1-yl)-2,2,2-trifluoro-ethanone

反応条件

後処理

1. 1
   その他the reaction liquid
2. 2
   抽出this was then extracted with ethyl acetate
3. 3
   洗浄The organic layer was washed with saturated saline
4. 4
   乾燥dried with anhydrous sodium sulfate
5. 5
   その他The solvent was evaporated away under reduced pressure
6. 6
   その他the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1)

実験手順

153 mg of potassium nitrate was added to a trifluoroacetic acid (2 ml) solution of 588 mg of 1-(2-(5-amino-2-(4-methanesulfonyl-phenoxy)-phenyl)-pyrrolidin-1-yl)-2,2,2-trifluoro-ethanone, and the reaction liquid was stirred overnight at room temperature. Aqueous saturated sodium bicarbonate was added to the reaction liquid to neutralize it, and this was then extracted with ethyl acetate. The organic layer was washed with saturated saline, 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=1/1) to obtain the entitled compound as a yellow solid.

出典