Biology Reference
In-Depth Information
9.5.3.3
Synthesis of the Rectangle 10
Complex
1
(12.1 mg, 0.01 mmol) and
N
-(4-pyridyl)isonicotinamide
(
6
; 2.0 mg, 0.01 mmol) were reacted in acetone to obtain
10
in
95% yield. Anal. calcd. (found) for C
H
N
O
P
Pt
: C, 45.07
106
158
10
14
8
4
(44.83); H, 5.63 (5.62); N, 4.96 (4.74). ESI-MS (
m
/
z
): 1349.12 [
10
3
-
3
-
3+
-1
- 2NO
]2+, 878.21 [
10
- 3NO
]
. IR data (KBr pellet,
ν
/cm
)
max
1
for
12.05
(s, 2H, NH), 9.2 (s, 2H, anthracene-H), 8.95 (d, 4H, pyridine-H),
8.46 (s, 2H, anthracene-H), 8.41-8.32 (m, 8H, pyridine-H), 7.92
(d, 4H, anthracene-H), 7.59 (m, 4H, anthracene-H), 7.43 (m, 4H,
anthracene-H), 7.34 (d, 4H, pyridine-H), 1.95 (q, 48H, -CH
10
: 2105 (C
∫
C), 1696 (C=O).
H NMR (CDCl
, 400 MHz):
δ
3
), 1.3 (t,
2
13
72H, -CH
).
C NMR (CH
NO
+ CDCl3):
δ
170.1 (2C, CO), 154.2 (8C,
6
),
3
3
2
152.2 (8C,
), 133.5 (8C, anthracene), 132.8 (4C, anthracene), 129.1
(4C, anthracene), 127.0 (8C, anthracene), 123.3 (4C, anthracene),
122.1 (4C, ethynyl), 119.4 (4C,
6
6
), 87.4 (4C, ethynyl), 15.9 (24C,
31
PEt
), 9.0 (24C, PEt
).
P NMR (CDCl
):
δ
14.98 and 13.91.
3
3
3
9.5.3.4
Synthesis of the Rectangle 11
Complex
1
(12.1 mg, 0.01 mmol) and
N
,
N
¢
-bis(4-pyridylidene)
ethylenediamine (
7
; 2.4 mg, 0.01 mmol) were reacted in acetone to
obtain
11
in 94% yield. Anal. calcd. (found) for C
H
N
O
P
Pt
:
112
164
12
12
8
4
C, 46.40 (46.24); H, 5.70 (5.78); N, 5.79 (5.65). ESI-MS (
m
/
z
):
3
-
2+
3
-
2+
1387.00 [
11
- 2NO
]
, 1269.14 [
11
- 2NO
- 2PEt
]
, 905.00 [
11
3
3
-
3+
3
-
3+
- 3NO
]
, 786.20 [
11
- 3NO
- 3PEt
]
. IR data (KBr pellet,
ν
/
3
max
-1
∫
1
cm
δ
9.22 (s, 2H, anthracene-H), 8.9 (d, 8H, pyridine-H), 8.5 (s, 4H, =CH),
8.48 (s, 2H, anthracene-H), 8.09 (d, 4H, anthracene-H), 7.92 (d, 8H,
pyridine-H), 7.5 (d, 4H, anthracene-H), 7.4 (m, 4H, anthracene-H), 4.2
(s, 8H, CH
) for
11
: 2105 (C
C), 1600 (C=N).
H NMR (CD
OD, 400 MHz):
3
13
), 1.93 (q, 48H, PCH
), 1.2 (t, 72H, PCH
).
C NMR (CH
NO
2
2
3
3
2
), 133.5 (8C, anthracene), 132.8
(4C, anthracene), 128.3 (4C, anthracene), 127.0 (8C, anthracene),
123.2 (4C, anthracene), 122.2 (4C, ethynyl), 119.6 (4C,
+ CDCl
):
δ
154.4 (8C,
7
), 152.1 (8C,
7
3
7
), 111.5 (4C,
7
), 87.4 (4C, ethynyl), 61.0 (4C,
7
), 15.9 (24C, PEt
), 9.0 (24C, PEt
).
3
3
31
1
P NMR (CD
OD):
δ
14.42 (s,
J
= 2872 Hz).
3
Pt-P
9.5.3.5
Synthesis of the Macrocycle 13
In a 4 mL glass vial equipped with magnetic stir bar was taken solid
3
(24.1 mg, 0.023 mmol) and added minimum amount of MeOH required
to dissolve the solid. The same molar ratio of disodiumfumarate (3.7
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