反应详情

To a solution of (3,4-dimethyl-phenyl)-[2-(6-trifluoromethyl-pyridin-3-yl)-ethyl]-amine (500 mg, 1.70 mmol, as described in example 1, step 3) in CH2Cl2 (15 mL) was added under a nitrogen atmosphere at 0° C. (4-fluoro-phenyl)-oxo-acetic acid (300 mg, 1.78 mmol, commercially available) and EDC (342 mg, 1.78 mmol). After stirring for 12 h a ambient temperature, the mixture was washed with aqueous Na2CO3 (saturated, 15 mL) and water (15 mL), the combined aqueous layers were extracted with CH2Cl2 (3×15 mL) and the combined organic layers dried over sodium sulfate. Concentration and purification by chromatography (SiO2, heptane:ethyl acetate=95:5 to 60:40) afforded the title compound (527 mg, 70%) as a light yellow oil.

1. washthe mixture was washed with aqueous Na2CO3 (saturated, 15 mL) and water (15 mL)
2. extractionthe combined aqueous layers were extracted with CH2Cl2 (3×15 mL)
3. dry with materialthe combined organic layers dried over sodium sulfate
4. concentrationConcentration and purification by chromatography (SiO2, heptane:ethyl acetate=95:5 to 60:40)