تفاعل #1095840
ord-4017f5970f0b41a1af1bac5700e2c726
معادلة التفاعل
ظروف التفاعل
المعالجة
- 1أخرىEthanol was removed
- 2استخلاصthe reaction solution was extracted two times with chloroform
- 3غسيلThe extract was washed two times with water
- 4تجفيفThe organic phase was dried over Na2SO4
- 5أخرىthe solvent was removed
- 6أخرىThe residue was purified by column chromatography (HexH:AcOEt=4:1)
الإجراء التجريبي
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.