反应详情

To a stirred solution of (S)-5-oxo-pyrrolidine-2-carboxylic acid tert-butyl ester (740 mg, 4 mmol) in N,N-dimethylformamide (5 mL) sodium hydride (180 mg of 60% dispersion in mineral oil, 4.5 mmol) is added at room temperature. After 10 minutes, 3-chloro-2-fluoro-5-trifluoromethylpyridine (1 mL, 8 mmol) is added and the suspension stirred at room temperature. After 3 h the reaction mixture is treated with saturated ammonium chloride solution (150 mL), extracted with dichloromethane (2×100 mL). Combined extracts washed with brine (2×50 mL), water, dried over anhydrous Na2SO4 and solvent removed in vacuo. The crude is purified by chromatography over silica gel eluting with hexanes/ethyl acetate to give the title compound, ESI m/z 365 [M+H]+.

1. extractionextracted with dichloromethane (2×100 mL)
2. washCombined extracts washed with brine (2×50 mL), water
3. dry with materialdried over anhydrous Na2SO4 and solvent
4. customremoved in vacuo
5. customThe crude is purified by chromatography over silica gel eluting with hexanes/ethyl acetate