反应详情

4.27 g (0.013 mol) of ethyl 3,3′,4,4′-tetrafluorobenzilate 3c, 1.81 g (0.013 mol) of tropenol and 0.03 g sodium are heated as a melt at 75 mbar for 4 hours over a bath of boiling water, shaking from time to time. After cooling, the sodium residues are dissolved with acetonitrile, the solution is evaporated to dryness, and the residue extracted with dichloromethane/water. The organic phase is washed with water, dried over MgSO4, and evaporated to dryness. The residue remaining is mixed with diethylether/petroleum ether (1:9), suction filtered and washed. Yield: 2.50 g (46% of theory); TLC: Rf value: 0.29 (eluent: sec-butanol/formic acid/water (75:15:10)); melting point: 147° C.-148° C.

1. temperatureAfter cooling
2. customthe solution is evaporated to dryness
3. extractionthe residue extracted with dichloromethane/water
4. washThe organic phase is washed with water
5. dry with materialdried over MgSO4
6. customevaporated to dryness
7. additionThe residue remaining is mixed with diethylether/petroleum ether (1:9), suction
8. filtrationfiltered
9. washwashed