Cross polarization, magic angle <sup>13</sup>C NMR spectroscopy of poly(p‐phenylene) and lower oligomers

Brown, Charles Eric; Jones, Martin B.; Kovacic, Peter

doi:10.1002/pol.1980.130181002

Cited by 38 publications

(7 citation statements)

References 9 publications

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“…Prior work has shown that increasing chain length in the poly(p-phenylene) series results in higher spin densities in ESR. 15 As expected, the cases ( C G H G -A~C~~-C U C~~,~~J~ C~H G -S~C~& U C~~,~~ C G H G -M O C~~~~) in which the IR para band positions corresponded closely (802-805 cm-') also displayed similar spins/g in ESR (ca. 2 X 10l8).…”

Section: Ppp From Benzene and Catalyst-oxidant Systemssupporting

confidence: 75%

Properties of poly(p‐phenylene)s and the perdeuterated analog

Hsing

Khoury

Bezoari

et al. 1982

J. Polym. Sci. Polym. Chem. Ed.

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ESR data for poly(p‐phenylene) (PPP) prepared from benzene and catalyst‐oxidant systems were compared with data for PPP obtained by a variety of other methods. The results were similar, except for the Yamamoto preparation, and comparable to the spin densities for heterocyclic polymers of thiophene, pyrrole, and selenophene. Deuterated PPP from C6D6 showed significant differences in properties, in comparison to ordinary PPP, in relation to molecular weight, color, solubility, and spins/g in electron spin resonance (ESR). The implications are discussed with regard to the mechanism of benzene polymerization by AlCl3‐CuCl2.

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Section: Ppp From Benzene and Catalyst-oxidant Systemssupporting

confidence: 75%

Properties of poly(p‐phenylene)s and the perdeuterated analog

Hsing

Khoury

Bezoari

et al. 1982

J. Polym. Sci. Polym. Chem. Ed.

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“…In 1980, the first NMR spectrum (13C) of PPP was obtained via cross polarization, magic angle spinning (CP/MAS) techniques. 243 Since that time, other 13C NMR227,236,244,245 and lH NMR246 studies have been reported.…”

Section: Nmrmentioning

confidence: 99%

Dehydro coupling of aromatic nuclei by catalyst-oxidant systems: poly(p-phenylene)

Kovacic¹,

Jones²

1987

Chem. Rev.

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464

327

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“…Some of our findings have been reported in preliminary form. 21 Dehydrogenative coupling of biphenyl by aluminum chloride-cupric chloride in o-dichlorobenzene gave mainly p-sexiphenyl along with p-quaterphenyl and higher molecular weight products. p -Terphenyl was oligomerized in similar fashion to yield predominantly the dimer-type product p-sexiphenyl plus higher, uncharacterized oligomers.…”

Section: Esr Studiesmentioning

confidence: 99%

Oligomers from biphenyl, biphenyl‐d₁₀, or p‐terphenyl with aluminium chloride‐cupric chloride: Mechanism, ESR, and conductivity

Hsing

Kovacic

Khoury

1983

J. Polym. Sci. Polym. Chem. Ed.

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Biphenyl and biphenyl‐d10 were coupled by aluminum chloride‐cupric chloride. For the two systems, the yields of p‐quaterphenyl, p‐sexiphenyl, and sublimation residue were compared. The results, which have mechanistic significance, are similar to those reported earlier for benzene versus benzene‐d6; that is, a decrease in DP for the deuterated substrate. p‐Sexiphenyl, obtained from biphenyl or p‐terphenyl and aluminum chloride‐cupric chloride, displayed a concentration of 3 × 1017 spins/g in ESR. There was little or no change in spin density after sublimation or crystallization. Even after drastic purification by a variety of techniques the radical character persisted. Biphenyl was polymerized by aluminum chloride‐cupric chloride at temperatures in the 50–155°C range. Processable polymers with m‐ and p‐phenylene linkages were produced. When doped with AsF5, the highest conductivity obtained was 7.3 × 10−2 Ω−1 cm−1.

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Cross polarization, magic angle ¹³C NMR spectroscopy of poly(p‐phenylene) and lower oligomers

Cited by 38 publications

References 9 publications

Properties of poly(p‐phenylene)s and the perdeuterated analog

Properties of poly(p‐phenylene)s and the perdeuterated analog

Dehydro coupling of aromatic nuclei by catalyst-oxidant systems: poly(p-phenylene)

Oligomers from biphenyl, biphenyl‐d₁₀, or p‐terphenyl with aluminium chloride‐cupric chloride: Mechanism, ESR, and conductivity

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Cross polarization, magic angle 13C NMR spectroscopy of poly(p‐phenylene) and lower oligomers

Cited by 38 publications

References 9 publications

Properties of poly(p‐phenylene)s and the perdeuterated analog

Properties of poly(p‐phenylene)s and the perdeuterated analog

Dehydro coupling of aromatic nuclei by catalyst-oxidant systems: poly(p-phenylene)

Oligomers from biphenyl, biphenyl‐d10, or p‐terphenyl with aluminium chloride‐cupric chloride: Mechanism, ESR, and conductivity

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Cross polarization, magic angle ¹³C NMR spectroscopy of poly(p‐phenylene) and lower oligomers

Oligomers from biphenyl, biphenyl‐d₁₀, or p‐terphenyl with aluminium chloride‐cupric chloride: Mechanism, ESR, and conductivity