反应详情

To 2.0 g (5.95 mmoles) of 1,1-bis(5-chloropyrid-2-yl)-2-(1H-1,2,4-triazol-1-yl)ethanol and 2.4 g (35.3 mmoles) of imidazole in 60 ml. of acetonitrile was added with stirring 2.1 g (17.65 mmoles) of thionyl chloride, the reaction mixture stirred for 2 hrs at room temperature and the solvent allowed to evaporate. Dilute sodium bicarbonate solution (30 ml) was added to the residue and the mixture extracted with ethyl acetate (3×50 ml). The combined extracts were dried over magnesium sulfate, concentrated to dryness and the residue chromatographed on 230-400 mesh silica gel using ethyl acetate-petrol (b.p. 60°-80° C.) (1:1, v:v) as the eluent. The fractions containing the product were combined and concentrated in vacuo to a colorless oil. Treatment of the residue with ethereal hydrogen chloride gave 1.4 (60% yield) of the desired product as a white solid, m.p. 115°-125° C.

1. customto evaporate
2. additionDilute sodium bicarbonate solution (30 ml) was added to the residue
3. extractionthe mixture extracted with ethyl acetate (3×50 ml)
4. dry with materialThe combined extracts were dried over magnesium sulfate
5. concentrationconcentrated to dryness
6. customthe residue chromatographed on 230-400 mesh silica gel
7. additionThe fractions containing the product
8. concentrationconcentrated in vacuo to a colorless oil