反应详情

温度

60 °C

Iodine (13.3 g) was added to a mixed solution of 4-[1,1,1,3,3,3-hexafluoro-2-(methoxymethyl)oxypropan-2-yl]-2-propylphenol (3.63 g, 10.5 mmol) in pyridine (50 mL) at room temperature, followed by heating in an oil bath at an external temperature of 60° C. overnight. A 1 mol/L sodium thiosulfate aqueous solution was added to the reaction solution at room temperature, followed by extraction with ethyl acetate-water. The organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1) to obtain 4.20 g of the title compound (yield: 85%) as a brown solid.

1. extractionfollowed by extraction with ethyl acetate-water
2. concentrationThe organic layer was concentrated under reduced pressure
3. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1)