反应详情

温度

-10 °C

37.4 g of decafluorobiphenyl (0.112 mol) are dissolved in 700 ml of dimethylformamide, the mixture is cooled to −10° C. using a cryostat, and a solution of 29.8 g of potassium 4-benzyloxycarbonylphenoxide (0.112mol) in 300 ml of dimethylformamide is then added dropwise over the course of 2 hours. After 48 hours at −10° C., the potassium salt has reacted. The dimethylformamide is then removed in a rotary evaporator, the residue is taken up in a little tetrahydrofuran, and the solution is filtered through a silica-gel column. The clear solution obtained is evaporated in a rotary evaporator until a white solid precipitates out. The solid is then stirred in n-hexane, filtered off using a fluted filter and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet (yield: 92%).

1. customThe dimethylformamide is then removed in a rotary evaporator
2. filtrationthe solution is filtered through a silica-gel column
3. customThe clear solution obtained
4. customis evaporated in a rotary evaporator until a white solid
5. customprecipitates out
6. filtrationfiltered off
7. filtrationa fluted filter
8. customdried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum
9. customdrying cabinet (yield: 92%)