反应详情

To a −78° C. solution of 5-(4-Bromo-3-methyl-phenoxymethyl)-1-(2,6-dichloro-phenyl)-4-isopropyl-1H-pyrazole (906 mg, 2.0 mmol) in anhydrous THF is added 1.6 M n-butyllithium (1.35 mL). After 30 minutes, N,N-dimethylformamide is added (0.5 mL, 6.4 mmol). After 30 minutes, saturated aqueous ammonium chloride is added. The mixture is extracted with ethyl acetate (2×). The combined ethyl acetate layers are dried (MgSO4) and concentrated under reduced pressure. The crude residue is purified via flash chromatography (ethyl acetate/heptane gradient) to afford the title compound (110 mg, 14%). LC-ES/MS m/e 403.0 (M+1).

1. waitAfter 30 minutes
2. extractionThe mixture is extracted with ethyl acetate (2×)
3. dry with materialThe combined ethyl acetate layers are dried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. customThe crude residue is purified via flash chromatography (ethyl acetate/heptane gradient)