反应详情

IBX (9.03 g, 32.25 mmol) was added to 100 mL of DMSO, the resultant mixture was agitated at room temperature for 30 minutes, and then compound (64) (3.6 g, 8.062 mmol) was added thereto, and the resultant mixture was further agitated for 3 hours. The reaction mixture was filtered, 200 mL of water was added to a filtrate, and the resultant mixture was extracted with 100 mL of ethyl acetate three times. Combined organic layers were washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, and then dried over magnesium sulfate, and a solvent was distilled off by an evaporator. The residue was recrystallized from toluene, and thus 2-ethoxy-1,8-difluoro-7-((4-propylcyclohexyl)methoxy)phenanthrene-9,10-dione (65) (3.2 g, yield 34.5%) was obtained.

1. filtrationThe reaction mixture was filtered
2. addition200 mL of water was added to a filtrate
3. extractionthe resultant mixture was extracted with 100 mL of ethyl acetate three times
4. washCombined organic layers were washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine
5. dry with materialdried over magnesium sulfate
6. distillationa solvent was distilled off by an evaporator
7. customThe residue was recrystallized from toluene