反应详情

温度

20 °C

20 g (0.1 mol) of S-propyl dichlorothiophosphate are dissolved in 500 ml of hexane, and the solution is first treated, between 0° and -5° C., with 20 ml (0.14 mol) of triethylamine and then with 20 g (0.1 mol) of 2,2,3,3,4,4-hexafluorocyclopentan-1-ol, dissolved in 50 ml of methylene chloride. The mixture is stirred for 2 hours at 20° C., and ammonia is then passed in at 20° C. (DC check). To complete the reaction, the mixture is stirred for 24 hours at 20° C., the solid is filtered off, and the solvent is distilled off under reduced pressure. The residue is then purified further by filtration through silica gel (cyclohexane:ethyl acetate=7:3 parts by volume). After the solvent has been distilled off, 8.6 g (27% of theory) of O-(2,2,3,3,4,4-hexafluorocyclopentyl) S-propyl thiophosphoramidate of refractive index nD20 =1.4390 are obtained.

1. customis then passed in at 20° C. (DC check)
2. customthe reaction
3. stirringthe mixture is stirred for 24 hours at 20° C.
4. filtrationthe solid is filtered off
5. distillationthe solvent is distilled off under reduced pressure
6. filtrationThe residue is then purified further by filtration through silica gel (cyclohexane:ethyl acetate=7:3 parts by volume)
7. distillationAfter the solvent has been distilled off