反应详情

21.3 g of pentafluoronitrobenzene (0.1 mol) and 12 g of benzyl alcohol (0.11 mol, i.e. a 10% excess) are dissolved in 200 ml of dry γ-butyrolactone in a three-neck flask fitted with stirrer. 30 g of potassium carbonate (0.22 mol) are then added in portions, and the mixture is stirred at room temperature for 24 hours. The reaction solution is then filtered via a fluted filter, and the crude product is extracted by shaking with 200 ml of ethyl acetate and 300 ml of water. The organic phase is washed three times with water, dried over sodium sulfate and evaporated to half in a rotary evaporator. The reaction product crystallizes from the initially viscous solution. The precipitated reaction product is then recrystallized from a mixture of methylene chloride and petrol ether (volume ratio 1:1) and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet.

1. customfitted with stirrer
2. filtrationThe reaction solution is then filtered via
3. filtrationa fluted filter
4. extractionthe crude product is extracted
5. stirringby shaking with 200 ml of ethyl acetate and 300 ml of water
6. washThe organic phase is washed three times with water
7. dry with materialdried over sodium sulfate
8. customevaporated to half in a rotary evaporator
9. customThe reaction product crystallizes from the initially viscous solution
10. customThe precipitated reaction product
11. customis then recrystallized from a mixture of methylene chloride and petrol ether (volume ratio 1:1)
12. customdried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum
13. customdrying cabinet