Реакция #677819

ord-1bac611b9d77408f8d1b37e1104a652a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеA supply of BCTFB was obtained
  2. 2
    Другоеat 120° C.
  3. 3
    Другоеfor 4 hours
  4. 4
    workup.DISTILLATIONafter distillation under vacuum
  5. 5
    Температураin refluxing methanol for 15 hours

Методика

A supply of BCTFB was obtained by reacting ethylene with dibrominated CTFE in 1,1,1,3,3-pentafluorobutane at 120° C. for 4 hours using a mixture of tert-butyl peroxypivalate (TBPPi, 3 mol %) and 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane (Trigonox 101, 4.5 mol %) as radical initiators, with the resulting structure being Br—CF2—CFCl—CH2—CH2—Br after distillation under vacuum. This was dehydrochlorinated with KOH in refluxing methanol for 15 hours, forming Br—CF2—CFCl—CH═CH2 (BCTFB). Successful radical copolymerization of CTFE (96 mol % in the feed) with BCTFB initiated by TBPPi (2 mol % with respect to both monomers) was carried out at 74° C. in a 100 mL autoclave. The 19F NMR spectrum of the obtained polymer is shown in FIG. 7.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09234062B2uspto-grants-2016_01