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| To 3,5-bis(trifluoromethyl)aniline (1 mL, 6.4 mmol) in freshly distilled triethylamine (2.7 mL, 19.2 mmol) at 0 ºC was added phosphorous(V) oxychloride (179 ¦ÌL, 1.9 mmol) dropwise. The reaction was heated to reflux for 16 hours to give a red solid. The solid was dissolved CH2Cl2 (50 mL), washed with sat. aq. NH4Cl (3 ¡Á 100 mL) and the organic phase washed with brine (100 mL), dried (MgSO4) and the solvent removed in vacuo. Purification by flash column chromatography (10% EtOAc/Hexane) furnished the target compound. (304 mg, 0.42 mmol, 22%) as a pale yellow solid. Spectra consistent with reported data. |
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