反应详情

Under a nitrogen atmosphere, a DMF (50 mL) solution of compound (85) (10.0 g, 3.45 mmol), 3-ethyl-5-(2-hydroxyethyl)-4-methylthiazole-3-iumbromide (1.74 g, 6.89 mmol) and triethylamine (1.05 g, 10.34 mmol) was agitated at 60° C. for 6 hours. The reaction mixture was quenched with 150 mL of water, and extracted with 50 mL of dichloromethane three times. Combined organic layers were washed with a 1N hydrochloric acid aqueous solution, water and saturated brine, and then dried over magnesium sulfate, and a solvent was distilled off by an evaporator. The residue was washed with toluene, and thus 2-ethoxy-1,8-difluorophenanthrene-9,10-dione (86) (7.0 g, yield 70.5%) was obtained.

1. customThe reaction mixture was quenched with 150 mL of water
2. extractionextracted with 50 mL of dichloromethane three times
3. washCombined organic layers were washed with a 1N hydrochloric acid aqueous solution, water and saturated brine
4. dry with materialdried over magnesium sulfate
5. distillationa solvent was distilled off by an evaporator
6. washThe residue was washed with toluene