Issue in Honor of Prof Nicolò Vivona ARKIVOC 2009 (viii) 212-221
17
O vs
13
C NMR chemical shifts as effective indicators
of π-electron-density distribution
in hindered methyl benzoates
Massimo Maccagno,
a
Andrea Mele,
b
Roberta Musio,
c
Giovanni Petrillo,
a
Fernando Sancassan,
a
* Oronzo Sciacovelli,
c
and Domenico Spinelli
d
*
a
Dipartimento di Chimica e Chimica Industriale, Via Dodecaneso 31, I-16146 Genova
b
Dipartimento di Chimica, Materiali e Ingegneria Chimica ‘Giulio Natta’ del Politecnico, Via
Mancinelli 7, I-20131 Milano
c
Dipartimento di Chimica, Via Orabona 4, I-70126 Bari
d
Dipartimento di Chimica ‘G. Ciamician’, Via Selmi 2, I-40126 Bologna
E-mail: domenico.spinelli@unibo.it
Dedicated to Prof. Nicolò Vivona on his 70th birthday
Abstract
17
O NMR Substituent Chemical Shift (SCS) values on the carbonyl and methoxy oxygens in
methyl 2,6-dimethyl-4-X-benzoates 2’ have been measured in acetonitrile-d
3
and compared with
those of the 2,6-unsubstituted methyl 4-X-benzoates 2, the former exhibiting very little
sensitivity to the effect of 4-substituents and not appearing to be related to π-electron density
changes in such sterically hindered systems.
Conversely
13
C NMR SCS values of the methoxy carbon of the ester function in either 2 and 2’,
although modest in size, exhibit a very good dual substituent parameter (DSP) correlation with
the polar and resonance effect of 4-substituents and are therefore effective indicators of local π-
electron densities.
Moreover,
13
C NMR SCS values of the methoxy carbon of 2’ exhibit an excellent linear
correlation with those of 2,6-unsubstituted benzoates 2. Once more this agrees with our previous
conclusion that the resonance interaction between the aromatic ring and the ester group is
essentially related to a π-polarization effect, not involving charge-transfer between the two
moieties and therefore not sensitive to steric hindrance to their coplanarity.
Keywords:
17
O and
13
C NMR spectroscopy, alkyl benzoates, substituent effect
ISSN 1551-7012 Page 212
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ARKAT USA, Inc.