반응 #12072
ord-5458c1810da14b22b17018798e405eb9
용매
반응 조건
온도
-80°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.DISTILLATION200 ml of freshly distilled dry Et2O
- 2workup.ADDITIONis added to a 500 ml vessel (under an argon atmosphere)
- 3기타is kept below −60° C.
- 4workup.STIRRINGThe solution is stirred for over night
- 5온도to warm up to room temperature
- 6기타Formed red solution
- 7여과is filtered
- 8기타evaporated to dryness
실험 절차
200 ml of freshly distilled dry Et2O is added to a 500 ml vessel (under an argon atmosphere). The vessel is cooled down to −80° C. and 15 g (0.129 mol) of CF2═CFCl gas is bubbled to Et2O. 100 ml (0.13 mol) of sec-BuLi is added dropwise during three hours. The temperature of the solution is kept below −60° C. all the time. The solution is stirred for 15 minutes and 29 ml (27.08 g, 0.130 mol) of Si(OEt)4 is added in small portions. The solution is stirred for over night allowing it to warm up to room temperature. Formed red solution is filtered and evaporated to dryness to result crude trifluorovinyltriethoxysilane, CF2═CFSi(OEt)3.