反应详情

A stirred solution of 6-(3-pyridyl)-2-[1H]-quinolone (0.05 g) in DMF (0.5 cm3) was treated at room temperature with sodium hydride (0.012 g of a 50% dispersion in oil) for 1 hour. A solution of dimethyl sulphate (0.016 g) in DMF (0.2 cm3) was added and the mixture was stirred for 1.5 hours. The mixture was concentrated in vacuo, water (5 cm3) was added and the mixture was extracted with ethyl acetate (3×10 cm3). The combined organic extracts were dried (MgSO4), concentrated in vacuo and the residue chromatographed on silica (Merck "MK 60.9385") eluting with chloroform to yield a solid which was triturated with ether to afford 1-methyl-6-(3-pyridyl)-2-(1H)-quinolone 0.25H2O, m.p. 116°-118°, (0.02 g).

1. concentrationThe mixture was concentrated in vacuo, water (5 cm3)
2. additionwas added
3. extractionthe mixture was extracted with ethyl acetate (3×10 cm3)
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customthe residue chromatographed on silica (Merck "MK 60.9385")
7. washeluting with chloroform
8. customto yield a solid which
9. customwas triturated with ether