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J Fluoresc (2011) 21:149–159
phosphonate benzopheonone was obtained and went
directly to the next step with no further purification.
7.68(t, J=7.3 Hz, 3H, CHCHCH), 7.64 (d, J=8.0 Hz, 6H,
CCHCH), 7.58(t, J=7.0 Hz, 6H, CHCHCH), 7.32(m, J=
16.0 Hz, 6H, CCHCH), 7.11(d, J=8.0 Hz, 6H, CCHCH).
Anal. Calcd for C63H45NO3, C, 87.57, H, 5.25, N, 1.62,
O, 5.56, Found, C, 87.43, H, 5.19, N, 1.71.
4-N, N-diphenylamino-4′-phenacyl-stilbene (C1)
4-Phosphonate benzophenone (0.939 g, 3 mmol) reacted
with N, N-diphenyl-benzaldehyde (0.903 g, 3 mmol) in dry
THF using sodium ethoxide (1.7 g, 20 mmol) as base at
room temperature overnight. After the filtration of solid
materials and evaporation of THF in vacuum, the reactant
mixture was dissolved in chloroform and washed by water.
The organic layer was dried with anhydrous magnesium
sulphate. After evaporated in vacuum, C1 was purified with
column chromophgraphty using benzene as eluent, which
was further purified with recrystallization in methylene
chloride. C1: color: yellow, yield: 55%, m.p.: 49–51 °C,
1H-NMR (500 MHz, CDCl3, δ: ppm, J: Hz): 7.78(d, J=
7.0 Hz, 4H, CHCHC), 7.71(d, J=8.5 Hz, 2H, CHCHC), 7.65
(t, J=7.5 Hz, 1H, CHCHCH), 7.55(t, J=.8.5 Hz, 4H,
CCHCH), 7.31(t, J=8.0 Hz, 4H, CHCHCH), 7.22(d, J=
16.5 Hz, 2H, CCHCH), 7.08(t, J=7.3 Hz, 6H, CCHCH),
7.00(d, J=8.5 Hz, 2H, CHCHCH). 13C-NMR: (123.472,
124.887, 125.741, 126.118, 127.880, 128.484, 129.505
130.065, 130.943 131.046, 132.365, 135.983, 138.063,
142.067, 147.504, 148.150, 196.209). Anal. Calcd for
C33H25NO, C, 87.77, H, 5.58, N, 3.10, O, 3.54, Found,
C, 87.59, H, 5.69, N, 3.21.
Results and discussion
Synthesis
Formyl groups could be easily introduced to triphenylamine
with Vilsmeier reaction. While remarkably low yields of tri
(p-formylphenyl)yl-benzaldehyde were observed even if
much excess of POCl3/DMF were used. This is mostly
caused by the deactivation of the remaining benzene ring
by the imine groups on the other two phenyl groups in the
third formylation step. The reaction of 4-phosphonate
benzopheonone and p-amino-benzaldehyde easily occurred
using sodium ethoxide as base. Stronger base such as
sodium hydride led to more byproducts in the final step.
Owing to poor solubility in most of solvents caused by
excess phenyl rings of C2 and C3, the purification and
characterization had to be carried out carefully.
X-ray crystallographic analysis
4,4′-Di(4-benzoylphenylethylene)yl-triphenylamine
(C2)The reaction of N,N-diphenyl-benzaldehyde (0.452 g,
1.5 mmol) and 4-phosphonate benzopheonone (0.903 g,
3 mmol) was carried out in THF using sodium ethoxide
(1.7 g, 10 mmol) as base at room temperature. Purification
of C2 was the same as that of C1. C2: color: yellow, yield:
53%, m.p. 172–174 °C, 1H-NMR (CDCl3): 7.82(t, J=
6.8 Hz, 8H, CHCHC), 7.60(t, J=6.8 Hz, 6H, CHCHC),
7.50(t, J=7.5 Hz, 4H, CHCHCH),7.45 (d, J=8.5 Hz, 4H,
CCHCH), 7.31(t, J=7.8 Hz, 2H, CHCHCH), 7.21(d, J=
16.0 Hz, 2H, CCHCH), 7.16(d, J=8.0 Hz, 2H, CHCHC),
7.10(t, J=9.2 Hz, 6H, CCHCH). 13C-NMR: (123.986,
125.332, 126.18, 127.9721, 128.435, 129.650, 130.083,
130.956 131.440, 132.405, 136.123, 138.50, 141.961,
147.114, 147.628, 196.228). Anal. Calcd for
C48H35NO2, C, 87.64, H, 5.36, N, 2.13, O, 4.86, Found,
C, 87.55, H, 5.279, N, 2.03.
The asymmetric unit contains one crystallographically
unique organic product, one propa-1, 2-diene molecule
and one solvent molecule, benzene (Fig. 2). Crystallo-
graphic disorder of single crystal of C1 induce that two
carbon have two positions ((C14), and C(14)′), (C(15), and
C(15)′), which have 50% rate of the occupancy respective-
ly. The organic product consists of five phenyl rings. As
shown in Figs. 2 and 3, rings 1–5 were composed of C
atoms from C2 to C7, C8 to C13, C16 to C21, C22 to C27
and C28 to C33, respectively. Rings 1 and 3 are almost
coplanar (Dihedral angle: 16.3°). The dihedral angles
between planes 1 and 2, 2 and 4, 2 and 5 were 58°, 61.8°
and 69.1°, respectively. X1 and X2 are the centers of rings
2 and 4. The X1⋯H27A and X2⋯H33B distance are
3.194 Å and 3.007 Å, respectively (atom with additional
labels A, B refers to the symmetry operations. A: x−1, 1.5−y,
0.5+z; B: x, 1.5−y, z−0.5), indicating strong edge-to-face π–π
stacking interactions existed (Fig. 3).
4,4′,4″-Tri(4-benzoylphenylethylene)yl-triphenylamine
(C3) The reaction of di(p-formylphenyl)yl-benzaldehyde
(0.330 g, 1 mmol) and 4-phosphonate benzopheonone
(0.903 g, 3 mmol) was performed in dry THF containing
sodium ethoxide (1.7 g, 20 mmol) for overnight at room
temperature. The purification was carried out as that of C1
and C2. C3: color: yellow, yield: 50%, m.p.:171–172 °C,
1H-NMR (d6-DMSO): 7.75(d, J=10.5 Hz, 18H, CHCHC),
UV/visible absorption spectroscopy
Due to electron-withdrawing effect of carbonyl group in
benzophenone unit and electron-donating effect of N core,
the derivatives exhibit typical D-π-A character. As shown
in Fig. 4, a gradual red-shift of the maximal absorption