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mg, 0.023 mmol) dissolved in minimum amount of water was added
to the above solution. Yellow precipitate was formed in a few minutes.
After 2 h of stirring the yellow solid was collected by centrifugation,
washed with methanol and dried under vacuum to get
13
as yellow
powder with good yield. Microcrystalline
was obtained from slow
evaporation of chloroform or dichloromethane
13
solution. Anal. calcd.
for C
H
O
P
Pd
: C 53.97, H 6.89. Found: C
53.51, H 7.00. MALDI-
92
140
8
8
4
MS: 2045.5 (13%) [
13
+ H
+
]; Q-TOF-ESI: 1691.66
(100%) [
13
+ H
+
1
- 3PEt
(s, 1H), 8.41 (s,
1H), 7.86 (d, 2H), 7.52 (d, 2H), 7.42-7.40 (m, 2H), 2.1-2.00 (m, 24H),
1.37-1.23 (m, 36H).
];
H NMR (400 MHz; CDCl
):
δ
/ppm = 9.47
3
3
31
1
P{
H} NMR (CDCl
, 121.4 MHz)
δ
/ppm: 17.31
3
13
1
(s).
C{
H}(CDCl
)
δ/
ppm: 172.63 (C
, fumarate carboxylate), 139.81
3
a
(C
, fumarate ), 136.03 (C
, anthracene), 132.45 (C
,
anthracene),
b
10
9
129.94 (C
, anthracene), 127.50 (C
, anthracene), 126.86 (C
,
1
11
12
anthracene), 126.15 (C
, anthracene), 125.59 (C
, anthracene),
2
4
125.03 (C
, anthracene), 106.24 (C
, ethynyl), 102.71 (C
, ethynyl),
¢
¢
3
2
1
∫
-1
20.44 (CH
-CH
-), 9.09 (CH
-CH
-). IR(KBr):
ν
(C
C) = 2103 cm
.
3
2
3
2
UV-vis
(CHCl
)
l
/nm (
e
/cm
-1
M
-1
): 279 (22250), 400 (5334),
3
max
424 (4518).
9.5.3.6
Synthesis of 4,4
¢
,4
¢¢
-Tris[Ethynyl-
Trans
-Pt(PEt
3
)
2
(NO
3
)]
Triphenylamine (14)
In a flame-dried Schlenk flask
N
,
N
,
N
-tris(4-ethynylphenyl)amine
[1.0 gm, 1.45 mmol] were
taken and the flask was degassed and purged with nitrogen. Then, 25
mL of dry, deoxygenated toluene and 10 mL of dry diethylamine were
added successively. After stirring for 30 min under N
[98.9 mg, 0.312 mmol] and
trans
-Pt(PEt
)
I
3
2
2
, CuI [25 mg,
0.132 mmol] was added and the mixture was stirred for 20 h under
N
2
Cl) was
separated and the solvent was removed under vacuum. The residue
was chromatographed using silica gel column by benzene/hexane
(1:1)
. The precipitated diethylammoniumchloride (Et
NH
2
2
2
¢
¢¢
(I)]
triphenylamine (400 mg) as pale yellow powder in 64% isolated
yield.
mixture
to
obtain
4,4
,4
-tris[ethynyl-
trans
-Pt(PEt
)
3
2
1
H NMR (CDCl
, 400 MHz):
δ
7.1 (d, 6H, Ph-H), 6.9 (d, 6H,
3
31
1
Ph-H), 2.2 (q, 36H, PEt
), 1.2 (t, 72H, PEt
).
P{
H} NMR (CDCl
, 120
3
3
3
MHz):
= 2874 Hz).
To a methanolic solution of AgNO
δ
8.6 (s,
1
J
P-Pt
[5.1 mg, 0.03 mmol] the
3
¢
¢¢
solution
of
4,4
,4
-tris[ethynyl-
trans
-Pt(PEt
)
(I)]triphenylamine
3
2
[19.9 mg, 0.01 mmol] in CHCl
was added. After stirring for 1 h the
yellowish precipitate of AgI was filtered through celite. Thus,
3
14
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