反应详情

温度

-20 °C

4 g (0.02 mol) of 2,2,3,3,4,4-hexafluorocyclopentan-1-ol, dissolved in 50 ml of tetrahydrofuran, are treated, at -70° C., with 8 ml of a 2.5-molar butyllithium solution in hexane. The mixture is heated to -20° C. and 5 g (0.02 mol) of O-ethyl S-propyl chlorothiophosphate are then added dropwise. To complete the reaction, the mixture is stirred for 24 hours at 20° C., a little water is added to the reaction mixture, and the mixture is filtered through silica gel. After the solvent has been distilled off and the residue has been distilled, 1.6 g (22% of theory) of O-ethyl O-(2,2,3,3,4,4-hexafluorocyclopentyl) S-propyl thiophosphate of a boiling point of b.p.0.15 90°-92° C. are obtained.

1. customthe reaction
2. filtrationthe mixture is filtered through silica gel
3. distillationAfter the solvent has been distilled off
4. distillationthe residue has been distilled