反应详情

4-(3-Fluoro-4-trifluoromethyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (853 mg, 2.45 mmol) was stirred in a mixture of trifluoroacetic acid/dichloromethane (5 mL, 25% v/v) for 20 min at room temperature. The reaction mixture was combined with 25 mL of CH2Cl2 and was washed with sat'd NaHCO3 (2×10 mL) and brine. The resulting CH2Cl2 layer was dried over anhydrous Na2SO4 and was concentrated to yield crude amine. The product was further purified by silica gel chromatography (gradient eluent 0-10% MeOH in dichloromethane) to provide 4-(3-fluoro-4-trifluoromethyl-phenyl)-piperazine (473 mg, 78%). The product was used directly in step 3.

1. washwas washed with sat'd NaHCO3 (2×10 mL) and brine
2. dry with materialThe resulting CH2Cl2 layer was dried over anhydrous Na2SO4
3. concentrationwas concentrated
4. customto yield crude amine
5. customThe product was further purified by silica gel chromatography (gradient eluent 0-10% MeOH in dichloromethane)