反应详情

温度

20 °C

10 g (0.05 mol) of S-propyl dichlorothiophosphate are dissolved in 500 ml of hexane and to the solution there are first added, between 0° and -5° C., 10 ml (0.07 mol) of triethylamine, and then 10 g (0.052 mol) of 2,2,3,3,4,4-hexafluorocyclopentan-1-ol, dissolved in 25 ml of methylene chloride. The mixture is stirred for 2 hours at 20° C. and 5 g (0.11 mol) of ethylamine are then added dropwise to the reaction mixture at 20° C. 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, 8.5 g (47% of theory) of O-(2,2,3,3,4,4-hexafluorocyclopentyl) S-propyl N-ethylthiophosphoramidate of refractive index nD20 =1.4292 are obtained.

1. additionare first added, between 0° and -5° C.
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