DOI: 10.1039/C5NJ00582E
Page 5 of 15
New Journal of Chemistry
(
d, 4H, J=9.0 Hz, H ), 7.41 (d, 4H, J=9.0 Hz,
AgNO (0.17 g, 1.0 mmol) was added to an
3
13
H ), 7.47-7.51 (m, 2H, H ), 7.61-7.65(m, 2H, 35 ethanol solution of Ru(bpy) Cl ·2H O (0.26 g,
1
2
3
2
2
2
H ), 7.99 (d, 2H, J = 6.0 Hz, H ), 8.27 (d, 2H, J =
0.5 mmol). After refluxing for 30 min and
filtering to remove the deposited AgCl, the
filtrate was added to an ethanol solution of
8
4
9
.0 Hz, H ), 8.90 (d, 2H, J = 3.0 Hz, H ), 9.19 (d,
7 2
5
0
5
0
5
0
2H, J = 3.0 Hz, H9).
2
1-3
BL : C H N O (0.41 g, 64 %). Anal. Calc: C,
BL (0.25 mmol).The mixture was refluxed
4
1
34
6
2
7
5
2
6.64; H, 5.29; N, 13.08. Found: C, 76.71; H, 40 under the protection of nitrogen atmosphere for
-1
.31; N, 13.06%. IR (cm , KBr): 3285(N-H),
936(C-H), 1607(C=C), 1500(C=C), 1327(C-N),
24 h. After most of the solvent was removed
under a reduced pressure, an orange-red
precipitate was obtained by the dropwise
1
1
2
2
3
1046 (C-O-C), 823(C-H) (pyridine), 736(β-ring)
1
(
pyridine), 622(C-C). H NMR(300 MHz; CDCl ; addition of a 4-fold excess of saturated aqueous
3
2
4
2
98K): 2.29(m, 2H, -CH ), 4.21 (m, 4H, -O-CH ), 45 KPF solution. The purification was carried out
2
2
6
.49(s, 4H, -N-CH ), 4.70 (s, 2H, -NH), 6.75(s,
by column chromatography on neutral
2
H, H ), 6.95 (d, 4H, J=9.0 Hz, H ), 7.39 (d, 4H,
aluminium oxide with CH CN-H O-saturated
6
13
3
2
J=9.0 Hz, H ), 7.47-7.51 (m, 2H, H ),
aqueous KNO (10:3:1, v/v/v) as eluent followed
12
3
3
7
.60-7.64(m, 2H, H ), 7.99 (d, 2H, J = 9.0 Hz,
by reprecipitation with a saturated KPF aqueous
8
6
H ), 8.26 (d, 2H, J = 9.0 Hz, H ), 8.89 (d, 2H, J = 50 solution. Orange-red powder was obtained
4
7
3
.0 Hz, H ), 9.18 (d, 2H, J = 3.0 Hz, H ).
in >60% yields.
2
9
3
1
BL : C H N O (0.39 g, 59 %). Anal. Calc: C,
[Ru(bpy) -BL -Ru(bpy) ](PF ) , complex 1:
4
2
36
6
2
2
2
6 4
76.83; H, 5.49; N, 12.80. Found: C, 76.85; H,
Yield: 65%. Anal. Calcd for C H N O Ru
80 64 14 2 2
-1
5
2
1
.44; N, 12.90%. IR (cm , KBr): 3329(N-H),
(PF ) : C, 47.20; H, 3.15; N, 9.64. Found: C,
6 4
-1
936(C-H), 1593(C=C), 1500(C=C), 1291(C-N), 55 47.26; H, 3.14; N, 9.66. IR (cm , KBr):
032 (C-O-C), 816(C-H) (pyridine), 729(β-ring)
3329(N-H), 2936(C-H), 1593(C=C), 1500(C=C),
1
(
pyridine), 622(C-C). H NMR(300 MHz; CDCl ; 1291(C-N), 1032 (C-O-C), 816(C-H) (pyridine),
3
1
298K): 2.03(s, 4H, -CH ), 4.08 (s, 4H, -O-CH ),
729(β-ring) (pyridine), 622(C-C). H NMR (300
2
2
4
2
.50(s, 4H, -N-CH ), 4.64 (s, 2H, -NH), 6.77(s,
MHz; DMSO-d ; 298K): 4.00(s, 2H, -NH),
2
6
H, H ), 6.94 (d, 4H, J=9.0 Hz, H ), 7.40 (d, 4H, 60 4.26 (s, 4H, -O-CH ), 4.57(s, 4H, -N-CH ),
6
13
2
2
J=9.0 Hz, H ), 7.50-7.54 (m, 2H, H ),
6.87(s, 2H, H ), 6.94 (d, 4H, J=6.0 Hz, H ), 7.27
6 13
12
3
7
.60-7.64(m, 2H, H ), 8.00 (d, 2H, J = 6.0 Hz,
(d, 4H, J=9.0 Hz, H ), 7.37-7.44 (m, 4H, H , H ),
12 3 8
8
H ), 8.26 (d, 2H, J = 9.0 Hz, H ), 8.91 (d, 2H, J =
7.77-7.82(m, 12H, bpy), 7.95 (d, 2H, J = 9.0 Hz,
4
7
3
.0 Hz, H ), 9.19 (d, 2H, J = 3.0 Hz, H ).
H ), 8.08(m, 4H, bpy), 8.15(m, 4H, bpy), 8.19(d,
4
2
9
2
.2.2 Synthesis of dinuclear Ruthenium 65 4H, J = 9.0 Hz, bpy ), 8.26 (d, 2H, J = 9.0 Hz,
complexes 1-3
H ), 8.27(m, 4H, bpy), 8.81 (d, 2H, J = 3.0 Hz,
7
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