反应详情

温度

0 °C

Nickel chloride (3.0 mg) was added to THF (1 mL) under an argon atmosphere, and the mixture was kept at 0° C. To the mixture, a THF solution (0.38 mL) of 0.93 M bromomethylmagnesium was slowly added, and a THF solution (2 mL) of 2-chloro-4-(3,4,5-Trimethoxyphenyl)pyridine (50 mg) was then slowly added. The mixture was stirred at 0° C. for 10 minutes and then at 70° C. for 1.5 hours. A small amount was diluted hydrochloric acid was added to the reaction mixture at 0° C. to conduct extraction with ethyl acetate. The resultant organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (dichloromethane:methanol=15:1) to obtain the title compound.

1. customwas kept at 0° C
2. waitat 70° C. for 1.5 hours
3. additionwas added to the reaction mixture at 0° C.
4. extractionextraction with ethyl acetate
5. washThe resultant organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by column chromatography on silica gel (dichloromethane:methanol=15:1)