Synthesis of Trifluorovinyloxy Aryl Ether Monomers

Synthesis of Trifluorovinyloxy Aryl Ether Monomers 3.2.2.I. Method III 

Into a 500-ml five-necked flask fitted with a mechanical stirrer, a reflux condenser, and a thermocouple attached to a temperature controller is placed freshly activated granular zinc (4.3 g, 0.066 mol) and 25 ml dry acetonitrile. This mixture is stirred and heated to reflux (83 C) under nitrogen while the 2-bromotetrafluoroethoxy aryl product (amount corresponding to 0.021 mol equivalents of 2-bromotetr uoroethoxy functionality) is dissolved in 21 ml of acetonitrile and added dropwise. The resulting mixture is stirred at 85 C for 6h, then cooled and filtered. The filtrate is evaporated at 60°C under vacuum to remove the acetonitrile and the residue is purified by distributing the desired 

A sample of monomer ( 50 g) was placed in a 100-ml round bottomed flask, which was attached to a rotary evaporator. The flask was heated to 150°C with the aid of an oil bath while stirring under vacuum (0.20 mmHg). The monomer was stirred and heated under vacuitm for a period of 45 min to 1 h in order to simultaneously degas and B-stage the monomer. The B-staged monomer was then held under nitrogen and poitred into a preheated mold, which consisted of two polished aluminum plates (6 x 6 x 1/2 in.) with a three-sided 1/8-in. thick Teflon spacer between the two plates. The spaeer was cut from a 6 x 6 x 1/8 in. 

Fabrication of Polymer Film Samples for Thermal Stability Testing 

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