反应详情

n-BuLi (42 mL, 1.6M, 67 mmol) was added to a solution of 3-bromopyridine (5.9 mL, 9.74 g, 62 mmol) in ether (200 mL) at −78 C. The resulting yellow suspension was stirred for 1 h. A solution of nicotinaldehyde (5.3 mL, 6 g, 56 mmol) in ether (25 mL) was then added. After stirring for 0.5 h, the reaction mixture was allowed to warm gradually to 0 C. The reaction mixture was then quenched by addition of half saturated brine (100 mL). The resulting mixture was extracted once with ethyl acetate and once with chloroform. Drying (1:1 Na2SO4/K2CO3) and concentration gave dipyridin-3-ylmethanol as a very viscous orange oil which was used without further purification.

1. stirringAfter stirring for 0.5 h
2. temperatureto warm gradually to 0 C
3. customThe reaction mixture was then quenched by addition of half saturated brine (100 mL)
4. extractionThe resulting mixture was extracted once with ethyl acetate and once with chloroform
5. customDrying
6. concentration(1:1 Na2SO4/K2CO3) and concentration