反応 #1095840
ord-4017f5970f0b41a1af1bac5700e2c726
反応方程式
反応条件
後処理
- 1その他Ethanol was removed
- 2抽出the reaction solution was extracted two times with chloroform
- 3洗浄The extract was washed two times with water
- 4乾燥The organic phase was dried over Na2SO4
- 5その他the solvent was removed
- 6その他The residue was purified by column chromatography (HexH:AcOEt=4:1)
実験手順
To an ethanol solution (500 mL) of carbazole (2.50 g, 15.0 mmol), NaIO4 (0.80 g, 3.75 mmol) and I2 (1.89 g, 7.45 mmol) were sequentially added, and then an ethanol solution (100 mL) of H2SO4 (1.60 mL, 30.0 mmol) was added. The reaction solution was refluxed for one hour at 65° C. The loss of raw materials was confirmed by TLC (HexH:AcOEt=4:1), and an ethanol solution (100 mL) of NaOH (1.4 g) was added thereto to neutralize the system. Ethanol was removed, and then the reaction solution was extracted two times with chloroform. The extract was washed two times with water. The organic phase was dried over Na2SO4, and the solvent was removed. The residue was purified by column chromatography (HexH:AcOEt=4:1), and thus compound 1 (3.06 g, 70%) was obtained as a white powder. Thus, 3,6-diiodocarbazole (0.47 g, 7.5%) was obtained as a white powder.