反应详情

4'-Chloro-2-(1H-1,2,4-triazol-1-yl)propiophenone (2 g.) in dry tetrahydrofuran (30 ml) was added to a suspension of sodium hydride (480 mg. of a 60% dispersion in oil) in dry tetrahydrofuran (20 ml) at 0° under a nitrogen atmosphere. After stirring for 10 minutes, methyl iodide (2.28 g.) in dry tetrahydrofuran (10 ml.) was added dropwise and the reaction mixture was then stirred at 0° for 1 hour and then at room temperature overnight. The reaction mixture was then diluted with water (20 ml), extracted with ether (3×25 ml), and the combined organic extracts were washed with water and dried (MgSO4). The residue obtained after removal of the solvent was flash chromatographed on silica (150 g.) using ethyl acetate/hexane/diethylamine (50:50:3 v/v/v) for elution and the product-containing fractions on evaporation followed by crystallisation of the residue from ethyl acetate/hexane furnished the title compound, (1.68 g., 84% yield), m.p. 118°-9°.

1. customat 0°
2. stirringthe reaction mixture was then stirred at 0° for 1 hour
3. customat room temperature
4. customovernight
5. extractionextracted with ether (3×25 ml)
6. washthe combined organic extracts were washed with water
7. dry with materialdried (MgSO4)
8. customThe residue obtained
9. customafter removal of the solvent
10. customchromatographed on silica (150 g.)
11. washfor elution
12. customthe product-containing fractions on evaporation
13. customfollowed by crystallisation of the residue from ethyl acetate/hexane