反应详情

温度

40 °C

A mixture of 4-(3-aminophenyl)-8-(trifluoromethyl)quinoline-3-carbonitrile (0.30 g, 0.96 mmol), 30% hydrogen peroxide (5 mL), NaOH (0.5 g, 12 mmol) and ethanol (15 mL) was heated to ˜40° C. for 3 hours. The pH of the solution was adjusted to ˜6 by diluted HCl. The reaction mixture was partitioned between ethyl acetate and water and the aqueous layer was extracted with ethyl acetate. The combined organic phases were washed with water, brine, and dried with magnesium sulfate. The organic phases were concentrated and the residue was loaded onto silica gel and chromatographed with hexanes:ethyl acetate (50% to 100%) to afford 0.13 g of the title compound as an off-white solid. MS (ESI) m/z 332;

1. customThe reaction mixture was partitioned between ethyl acetate and water
2. extractionthe aqueous layer was extracted with ethyl acetate
3. washThe combined organic phases were washed with water, brine
4. dry with materialdried with magnesium sulfate
5. concentrationThe organic phases were concentrated
6. customchromatographed with hexanes