反应详情

Under an argon atmosphere, a tetrahydrofuran solution (1.5 ml, 3 mmol) of isopropylmagnesium chloride was added dropwise to a tetrahydrofuran (2 ml) solution of 2-bromo-3-methoxypyridine (564 mg, 3 mmol) under ice cooling. The resulting mixture was stirred at room temperature for 60 minutes. Under ice cooling, 2,5-difluorobenzaldehyde (328 μl, 3 mmol) was added dropwise to the resulting brown solution. The temperature of the reaction mixture was raised gradually to room temperature. To the reaction mixture was added a saturated aqueous solution of ammonium chloride, followed by extraction with ethyl acetate. The solvent was dried, followed by concentration under reduced pressure to yield needle crystals. The resulting needle crystals were triturated with hexane, whereby the title compound (660 mg, 88%) was obtained.

1. temperatureThe temperature of the reaction mixture was raised gradually to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. customThe solvent was dried
4. concentrationfollowed by concentration under reduced pressure
5. customto yield needle crystals
6. customThe resulting needle crystals were triturated with hexane, whereby the title compound (660 mg, 88%)
7. customwas obtained