反应详情

Ethyl magnesium bromide (1.15 mmol, 3.0M in ethyl ether) is added drop-wise to a tetrahydro-furan (3 mL) solution of N-methoxy-N-methyl-2-(4′-trifluoromethyl-biphenyl-4-yl)-acetamide (0.248 g, 0.77 mmol) at −45° C. and stirred for one hour. Gradually raise temperature to −20° C. and stirred for one hour. The reaction is quenched by saturated ammonium chloride solution (1 mL) at 0° C., extracted with ethyl acetate and washed with water and brine. Organics are dried over sodium sulfate, filtered and concentrated. Column chromatography on silica gel with 0-30% ethyl acetate/hexane gradient gives 0.095 g (0.33 mmol, 42%) of the title compound.

1. stirringGradually raise temperature to −20° C. and stirred for one hour
2. customThe reaction is quenched by saturated ammonium chloride solution (1 mL) at 0° C.
3. extractionextracted with ethyl acetate
4. washwashed with water and brine
5. dry with materialOrganics are dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated