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Volumn 47, Issue 17, 2008, Pages 3279-3282

Visual observation of redistribution and dissolution of palladium during the Suzuki-Miyaura reaction

Author keywords

Cross coupling; Heterogeneous catalysis; Leaching; Palladium; Surface chemistry

Indexed keywords

DISSOLUTION; PALLADIUM;

EID: 53549131956     PISSN: 14337851     EISSN: None     Source Type: Journal    
DOI: 10.1002/anie.200800153     Document Type: Article
Times cited : (93)

References (29)
  • 2
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    • Eds, F. Diederich, P. J. Stang, Wiley-VCH, Weinheim
    • Metal-Catalyzed Cross-Coupling Reactions (Eds.: F. Diederich, P. J. Stang), Wiley-VCH, Weinheim, 1998.
    • (1998) Metal-Catalyzed Cross-Coupling Reactions
  • 7
    • 53549095105 scopus 로고    scopus 로고
    • To the best of our knowledge, Pd foil has not been employed in coupling reactions, although it has been used in oxidation and reduction chemistry (see references [8-11]).
    • To the best of our knowledge, Pd foil has not been employed in coupling reactions, although it has been used in oxidation and reduction chemistry (see references [8-11]).
  • 12
    • 53549108762 scopus 로고    scopus 로고
    • The morphology of the surface is identical to that which has not been treated with any solvents or reagents
    • The morphology of the surface is identical to that which has not been treated with any solvents or reagents.
  • 16
    • 53549101538 scopus 로고    scopus 로고
    • No change in the surface was observed if the Pd was exposed to the boronic ester component alone (see Figure S-1 in the Supporting Information).
    • No change in the surface was observed if the Pd was exposed to the boronic ester component alone (see Figure S-1 in the Supporting Information).
  • 17
    • 53549096139 scopus 로고    scopus 로고
    • XPS data were also obtained in the B1s region, but in no case was any signal detected. C1s and O1s spectra were also obtained but were mostly unremarkable; for the C1s region, they showed a single peakat a binding energy of 285.0 eV. The O1s spectra consisted of a single peakat binding energy of 532.6 eV in all cases. Both are likely due to trace contaminants on the surface as they are present in all samples.
    • XPS data were also obtained in the B1s region, but in no case was any signal detected. C1s and O1s spectra were also obtained but were mostly unremarkable; for the C1s region, they showed a single peakat a binding energy of 285.0 eV. The O1s spectra consisted of a single peakat binding energy of 532.6 eV in all cases. Both are likely due to trace contaminants on the surface as they are present in all samples.
  • 18
    • 53549097246 scopus 로고    scopus 로고
    • 3/2 signal.
    • 3/2 signal.
  • 22
    • 53549103205 scopus 로고    scopus 로고
    • The as-received foil before extensive washing with DMF showed strong signals in the C1s and O1s spectra, indicative of the presence of a considerable amount of oxide and carbonaceous contaminants on the surface, in addition to a peak assignable to Pd oxide. Except for some small residual C1s and O1s signals, these all disappeared after the samples had been washed with DMF.
    • The as-received foil before extensive washing with DMF showed strong signals in the C1s and O1s spectra, indicative of the presence of a considerable amount of oxide and carbonaceous contaminants on the surface, in addition to a peak assignable to Pd oxide. Except for some small residual C1s and O1s signals, these all disappeared after the samples had been washed with DMF.
  • 23
    • 0001001387 scopus 로고    scopus 로고
    • It should be noted that poorly resolved XP spectra can be easily overfit to more peaks than the data warrant. However, if spectrum B is fit with only two peaks, the best fit is obtained with peaks of full width half maximum (FWHM) of 1.2 and 2.1 eV. This does not seem physically reasonable, as the FWHM for all other Pd spectra studied here was (1.5±0.2) eV. By fitting three peaks, the FWHM values become consistent with those for other spectra observed here and also by Takasu et al., who report values of 1.6 eV: Y. Takasu, R. Unwin, B. Tesche, A. M. Bradshaw, Surf. Sci. 1978, 77, 219.
    • It should be noted that poorly resolved XP spectra can be easily "overfit" to more peaks than the data warrant. However, if spectrum B is fit with only two peaks, the best fit is obtained with peaks of full width half maximum (FWHM) of 1.2 and 2.1 eV. This does not seem physically reasonable, as the FWHM for all other Pd spectra studied here was (1.5±0.2) eV. By fitting three peaks, the FWHM values become consistent with those for other spectra observed here and also by Takasu et al., who report values of 1.6 eV: Y. Takasu, R. Unwin, B. Tesche, A. M. Bradshaw, Surf. Sci. 1978, 77, 219.
  • 26
    • 0042136363 scopus 로고    scopus 로고
    • 2 spans a range of only 0.8 eV: S. W. Gaarenstroom, N. Winograd, J. Chem. Phys. 1977, 67, 3500.
    • 2 spans a range of only 0.8 eV: S. W. Gaarenstroom, N. Winograd, J. Chem. Phys. 1977, 67, 3500.
  • 28
    • 53549084763 scopus 로고    scopus 로고
    • To decrease reflection, the Pd surface needed to be coated with carbon black
    • To decrease reflection, the Pd surface needed to be coated with carbon black.


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.