SHORT COMMUNICATIONSConjugated polyphenylenes are used as materials for manufacture of display devices for electrophotography, illuminating equipment, photodetectors, sensors, field transistors, laser diodes, as well as heat-resistant polymeric materials [1,2]. At present, numerous methods for the synthesis of conjugated polyphenylenes from mono-and diacetylenic compounds and monoand diethynylarenes in the presence of metal complex or acid catalysts are known [3]. They were also synthesized from 1,3-and 1,4-dilithiobenzenes in the presence of tert-butyllithium [4], as well as by thermolysis of enediynes and dialkynylbenzenes [5], joint trimerization of mono-and difunctional acetylenes in the presence of TiCl 4 [6], and polycondensation of 1,4-and 1,3-dibromobenzenes [7].We have developed a simple procedure for the synthesis of previously unknown soluble diiodo-substituted polyphenylenes II on the basis of photochemical reaction (λ 254 nm) of 2-iodo-1-phenylethanone (I) in the absence of catalyst and solvent. After induction period (11 h at 80°C or 2 h at 140°C) the reaction occurred instantaneously with an appreciable exothermic effect (the mixture warmed up to 160°C). The reaction was accompanied by evolution of ethylene and carbon(II) oxide. In the IR spectrum of the gas mixture absorption bands at 1640 and 3100 cm -1 were present, which were assigned to stretching vibration of the C=C and C-H bonds in ethylene, and carbon(II) oxide gave rise to absorption at 2100 cm -1 .NMR monitoring of the reaction course showed that the key step is dehydrogenation of benzene rings with photochemically generated iodine radical, which favors polymerization process. The formation of hydrogen iodide as a result of dehydrogenation follows from the fact that the polymerization process (according to the NMR data) is accompanied by partial reduction of iodoacetophenone (I) to acetophenone: a signal assignable to methyl protons appeared in the 1 H NMR spectrum at δ 2.58 ppm, while in the 13 C NMR spectrum new signals at δ C 26.55 and 198.05 ppm were observed due to carbon nuclei in the CH 3 and C=O groups. Acetophenone and 2-chloro-1-phenylethanone did not change under analogous conditions (according to the NMR data).In the 1 H NMR spectrum of polyphenylene II, a multiplet in the region δ 7.27-8.30 ppm is typical of para-and/or meta-substituted benzene rings [1]. The IR spectrum of II contained specific narrow peaks in the region 830-841 cm -1 due to vibrations of para-substituted benzene rings [8]. Compound II displayed in the 13 C NMR spectrum signals from aromatic carbon atoms in the region δ C 135.66-120.90 ppm and signals at δ C 114.89 and 97.56 ppm, which may be assigned to aromatic carbon atoms attached to iodine. A strong IR band at 458 cm -1 corresponds to stretching vibrations of the C arom -I bond; it was identified using iodobenzene as model compound (448 cm -1 ). Polyphenylene II is paramagnetic (the concentration of paramagnetic species is 10 19 spin/g), and it showed in the ESR spectrum asymmetric singlets (asymmetry ...