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36
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2142789548
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Even scratches on the glass or a polished surface of a joint could promote this side reaction, so very smooth glassware or a plastic flask is recommended to minimize the by-product formation. For the same reason, it is difficult to use TLC to monitor the reaction (excessive colorization occurs when the reaction solution is put on a silica gel or alumina TLC plate).
-
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37
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24644518182
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A detailed investigation of the nucleophilic substitution in 9-dicyanomethylenepolynitrofluorenes with amines was described earlier: I. F. Perepichka, A. F. Popov, T. V. Orekhova, M. R. Bryce, A. N. Vdovichenko, A. S. Batsanov, L. M. Goldenberg, J. A. K. Howard, N. I. Sokolov, J. L. Megson, J. Chem. Soc. Perkin Trans. 2 1996, 2453-2470.
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38
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2142785705
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note
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Elemental analysis of the silica gel (LabPro, 40/60 for chromatography) gave K, 0.64%.
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39
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40
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2142722525
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note
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Unfortunately, the extremely low intensity of the CN peak in solution precludes a study of the solution IR behavior of this band.
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41
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2142740700
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note
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-1, which is due to overlap with the peak from the solvate molecule of MeCN.
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43
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2142787006
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note
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The assignment of the protons has been made by comparison with previously investigated fluorene derivatives and on the basis of a COSY experiment (for compound 15).
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0028417270
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45
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2142727633
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The same signal was observed for 16.
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46
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0033021850
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48
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2142735110
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2142837426
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note
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However, the values obtained to estimate the behavior of the molecule in solution should be used with caution since the solvation energy was not taken into account.
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60
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2142668471
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2142833667
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Appearance of the same bands was observed by electrochemical oxidation of TTF derivative 11 (Figure S7).
-
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66
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2142847576
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note
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The assignment of these bands is supported by spectroelectrochemical experiments on the fluorene derivative 6 (Figure S8) and the electronic spectra of isolated fluorene ion-radical salt 24.
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Perepichka, D.F.1
Bryce, M.R.2
Perepichka, I.F.3
Lyubchik, S.B.4
Christensen, C.A.5
Godbert, N.6
Batsanov, A.S.7
Levillain, E.8
McInnes, E.J.L.9
Zhao, J.P.10
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78
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2142731443
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note
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The yield could possibly be improved by using 5-10 times lower concentration.
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