反应详情

温度

-40 °C

To a solution of 2-bromo-5-[(2,5-difluorophenyl)[(3,5-difluorophenyl)thio]methyl]-4-methylpyridine (2.35 g, 5.31 mmol) in toluene (60 ml), a hexane solution of n-butyllithium (1.54 M, 4.14 ml, 6.38 mmol) was added in an argon atmosphere at −78° C. The reaction mixture was stirred for 30 minutes at −40° C., and then cooled again to −78° C., and N,N-dimethylformamide (0.494 ml, 6.38 mmol) was added. After completion of dropwise addition, the reaction mixture was Allowed to warm to 0° C., and water was added at the same temperature. Ethyl acetate was added to the reaction mixture, the organic layer was separated, and then the organic layer was washed with saturated brine. The organic layer was dried over anhydrous sodium sulfate and filtered, then the filtrate was concentrated under reduced pressure, and the obtained residue was subjected to flash silica gel chromatography. The fraction obtained from an elution with hexane:ethyl acetate=10:1 was concentrated under reduced pressure to obtain the title compound (1.36 g, 3.47 mmol, 65%) as a white solid.

1. temperaturecooled again to −78° C.
2. additionAfter completion of dropwise addition
3. temperatureto warm to 0° C.
4. customthe organic layer was separated
5. washthe organic layer was washed with saturated brine
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationthe filtrate was concentrated under reduced pressure
9. customThe fraction obtained from an elution with hexane
10. concentrationethyl acetate=10:1 was concentrated under reduced pressure