反应详情

The mixture of 2-fluoro-4-iodotoluene (0.05 mol), 3-methyl-3-hydroxy-1-butyne (0.06 mol), tetrakis (triphenylphosphonium) palladium (0) 0.35 g, copper iodide 50 mg, and diethylamine 100 ml was refluxed for 5.5 hours. Diethylamine was distilled away under reduced pressure, the residue was extracted with diethylether, and the extract was washed with water. From the extract, diethylether was distilled away, the residue was purified by column chromatography (elution liquid: heptane-ethyl acetate) to obtain colorless oily 2-fluoro-4-(3-methyl-3-hydroxy-1-butynyl)toluene (0.035 mol).

1. temperaturewas refluxed for 5.5 hours
2. distillationDiethylamine was distilled away under reduced pressure
3. extractionthe residue was extracted with diethylether
4. washthe extract was washed with water
5. distillationFrom the extract, diethylether was distilled away
6. customthe residue was purified by column chromatography (elution liquid: heptane-ethyl acetate)