反应详情

In 30 ml of ethanol were added 1.51 g (3.43 mmol) of 6-bromohexyl-[2,4-dichloro-5-(2,2,2-trifluoroethylthio)phenyl]ether and 1.67 g (17.2 mmol) of potassium thiocyanate. The mixture was refluxed for 3 hours under heating. The mixture was allowed to cool to room temperature, and the solvent was distilled off under reduced pressure. Then extraction was conducted by adding ethyl acetate and water. The organic phase obtained was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: a mixed solvent of n-hexane:ethyl acetate=10:1), to obtain 1.04 g (yield: 73%) of an intended product.

1. temperatureThe mixture was refluxed for 3 hours
2. temperatureunder heating
3. distillationthe solvent was distilled off under reduced pressure
4. extractionThen extraction
5. additionby adding ethyl acetate and water
6. customThe organic phase obtained
7. dry with materialwas dried over anhydrous magnesium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. customThe residue was purified by silica gel column chromatography (