Ethylene → 4-Bromo-3-chloro-3,4,4-trifluorobut-1-ene

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.

1. customA supply of BCTFB was obtained
2. customat 120° C.
3. customfor 4 hours
4. distillationafter distillation under vacuum
5. temperaturein refluxing methanol for 15 hours

ORD record

ord-1bac611b9d77408f8d1b37e1104a652a

Source dataset

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09234062B2