反応 #49286

反応方程式

water

trifluoroacetic acid

triethylsilane

4-Chloro-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone

→

4-chloro-7-iodoisoindolinone

収率 99.5%

溶媒

nitromethane

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with saturated brine
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   その他The solvent was evaporated under reduced pressure
5. 5
   その他the residue was purified by slurry

実験手順

4-Chloro-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (6.94 g, 16.2 mmol) was dissolved in nitromethane (280 mL), and the solution was added with trifluoroacetic acid (17.7 mL, 230 mmol) and triethylsilane (7.35 mL, 46.1 mmol), followed by stirring at room temperature for 23 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by slurry using diisopropyl ether to obtain 4-chloro-7-iodoisoindolinone (4.73 g, yield 99%).

出典