反应详情

温度

100 °C

To a 1,4-dioxane solution (30 ml) of 2,2,6,6-tetramethylpiperidine (3.11 g, 22.0 mmol) and potassium-bis(trimethylsilyl)amide (4.39 g, 22.0 mmol)2 was added 2,6-dibromopyridine (2.37 g, 10.0 mmol). The reaction mixture was stirred vigorously at 100° C. overnight. After cooling down to room temperature, the reaction was quenched with water and extracted with diethyl ether/THF (1:1) mixtures. The combined extracts were washed with 1 M Na2CO3, dried over MgSO4, filtrated, and evaporated to dryness. The product was purified by flash chromatography on silica gel leading to colorless oil (Rf=0.5 in Ethylacetate:hexane=1:20, Yield=1.13 g (31.6%))

1. temperatureAfter cooling down to room temperature
2. customthe reaction was quenched with water
3. extractionextracted with diethyl ether/THF (1:1) mixtures
4. washThe combined extracts were washed with 1 M Na2CO3
5. dry with materialdried over MgSO4
6. filtrationfiltrated
7. customevaporated to dryness
8. customThe product was purified by flash chromatography on silica gel leading to colorless oil (Rf=0.5 in Ethylacetate:hexane=1:20, Yield=1.13 g (31.6%))