تفاعل #12072

ord-5458c1810da14b22b17018798e405eb9

معادلة التفاعل

FC(F)=C(F)Cl
CF2═CFCl
[Li][CH](C)CC
sec-BuLi
CCO[Si](OCC)(OCC)OCC
Si(OEt)4
CCO[Si](OCC)(OCC)C(F)=C(F)F
CF2═CFSi(OEt)3

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
-80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATION200 ml of freshly distilled dry Et2O
  2. 2
    workup.ADDITIONis added to a 500 ml vessel (under an argon atmosphere)
  3. 3
    أخرىis kept below −60° C.
  4. 4
    workup.STIRRINGThe solution is stirred for over night
  5. 5
    درجة الحرارةto warm up to room temperature
  6. 6
    أخرىFormed red solution
  7. 7
    ترشيحis filtered
  8. 8
    أخرىevaporated to dryness

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07098346B2uspto-grants-2006_08