反応 #157995

反応方程式

2-Cyano-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]quinoline-6-carboxamide

urea hydrogen peroxide

trifluoroacetic anhydride

→

2-cyano-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]quinoline-6-carboxamide-1-oxide

収率 81.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   濃縮The reaction solution was concentrated under the reduced pressure
2. 2
   workup.DISSOLUTIONthe resulting residues were dissolved in ethyl acetate
3. 3
   洗浄The solution was washed with water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   ろ過The drying agent was filtered off
6. 6
   その他the solvent was removed by distillation under the reduced pressure
7. 7
   その他The resulting residues were purified by column chromatography

実験手順

2-Cyano-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]quinoline-6-carboxamide (240 mg) was dissolved in dichloromethane, added with urea-hydrogen peroxide adduct (85 mg) and trifluoroacetic anhydride (190 mg), and stirred at room temperature for 20 hours. The reaction solution was concentrated under the reduced pressure, and the resulting residues were dissolved in ethyl acetate. The solution was washed with water and dried over anhydrous magnesium sulfate. The drying agent was filtered off and the solvent was removed by distillation under the reduced pressure. The resulting residues were purified by column chromatography to obtain 2-cyano-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]quinoline-6-carboxamide-1-oxide (0.20 g, 81%).

出典