Chloroform → 4-(Dichloromethyl)-2-fluoro-5-nitrobenzotrifluoride

関与物質

反応手順

To a solution of potassium t-butoxide (1.25 g, 11.1 mmol) in tetrahydrofuran (25 ml) was slowly added dropwise a solution of 2-fluoro-5-nitrobenzotrifluoride (1.00 g, 4.78 mmol) and chloroform (599 mg, 5.02 mmol) in tetrahydrofuran (2.5 ml) at −78° C. After stirring for 15 minutes at the same temperature, acetic acid-methanol (1:1, 5 ml) was added and the temperature was raised to room temperature. Ethyl acetate and saturated brine were added to the reaction mixture, which was extracted with ethyl acetate. After washed with brine, the organic layer was dried over anhydrous magnesium sulfate and solvent was distilled off. The residue obtained was submitted to silica gel column chromatography [hexane→hexane-ethyl acetate(300:1)] to obtain 714 mg of title compound as pale yellow liquid. Yield 51%.

情報源と証拠