反应详情

A mixture of thiophene-2-thiol (1.5 mL), potassium carbonate (8.0 g) and N,N-dimethylformamide was treated dropwise with 2-fluorobenzaldehyde (1.7 mL), and the resulting mixture was stirred at room temperature for 42 hours. The mixture was treated with ice/water, extracted with ethyl acetate and the combined organic extract was dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel, eluting with a mixture of cyclohexane and ethyl acetate (1:0 to 9:1 by volume), followed by distillation at 50° C./11 mbar to afford the title compound as a red oil (1.9 g).

1. extractionextracted with ethyl acetate
2. extractionthe combined organic extract
3. dry with materialwas dried over magnesium sulfate
4. customThe solvent was removed under reduced pressure
5. customthe residue purified by column chromatography on silica gel
6. washeluting with a mixture of cyclohexane and ethyl acetate (1:0 to 9:1 by volume)
7. distillationfollowed by distillation at 50° C./11 mbar