反应详情

A solution of dipyridin-3-ylmethanone (1 g, 5.9 mmol) and 1-(4-fluorobenzyl)pyridin-2(1H)-one (1 g, 4.9 mmol) in THF (50 mL) was cooled to −78 C. To the resulting white suspension was added in a dropwise manner, LiHMDS (1M in THF, 6 mL). The resulting cream suspension was stirred for 30 min then allowed to warm up gradually to −30 C over 1 h. The reaction mixture was quenched with saturated NaHCO3 and then it was extracted once with ether and once with ethyl acetate. The combined extracts were dried over Na2SO4 and concentrated. The resulting yellow oil was purified by normal phase Gilson chromatography eluting with 98% DCM, 2% methanol. The product was isolated as a white solid.

1. temperatureto warm up gradually to −30 C over 1 h
2. customThe reaction mixture was quenched with saturated NaHCO3
3. extractionit was extracted once with ether and once with ethyl acetate
4. dry with materialThe combined extracts were dried over Na2SO4
5. concentrationconcentrated
6. customThe resulting yellow oil was purified by normal phase Gilson chromatography
7. washeluting with 98% DCM, 2% methanol
8. customThe product was isolated as a white solid