Biology Reference
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[16.9 mg] was obtained in 94% isolated yield after the removal of
the solvent. Anal. calcd. for C
H
N
O
P
Pt
: C, 40.16; H, 5.73; N,
60
102
4
9
6
3
3.12. Found: C, 40.29; H, 5.60; N, 3.23.
1
H NMR (CDCl
, 400 MHz):
3
δ
7.0 (d, 6H, Ph-H), 6.9 (d, 6H, Ph-H), 1.9 (q, 36H, PEt
), 1.2 (t, 72H,
3
31
1
1
PEt
).
P{
H} NMR (CDCl
, 120 MHz):
δ
20.0 (s,
J
= 3052 Hz).
3
3
P-Pt
9.5.3.7 1,1,1-Tris[4-(
Trans
-Pt(PEt
3
)
2
I)Ethynylphenyl]Ethane
In a flame-dried Schlenk flask 1,1,1-tris(4-ethynylphenyl)ethane
(120 mg, 0.363 mmol) and
(994.6 mg, 1.45 mmol)
were taken and degassed thrice followed by purging N
trans
-Pt(PEt
)
I
3
2
2
. Then, 30 mL
of dried and degassed toluene and 10 mL of dry diethylamine were
added and the mixture was stirred for 30 min before the addition
of CuI (20.0 mg, 0.105 mmol). Solvent was removed and the residue
was chromatographed using silica gel column chromatography
(1:1,
2
I)
ethynylphenyl]ethane (450 mg) was obtained as pale yellow powder
in 61% isolated yield after removal of the solvent. Anal. calcd. for
C
benzene/hexane).
Then,
1,1,1-tris[4-(
trans
-Pt(PEt
)
3
2
1
H
I
P
Pt
: C, 37.19; H, 5.29. Found: C, 37.47; H, 5.56.
H NMR
62
105
3
6
3
(CDCl
, 400 MHz):
δ
7.1 (d, 6H, Ph-H), 6.9 (d, 6H, Ph-H), 2.2 (q, 36H,
3
PEt
), 2.0 (s, 3H, CH
), 1.1 (t, 54H, PEt
).
31
P{
1
H} NMR (CDCl
, 120
3
3
3
3
1
MHz):
δ
8.5 (s,
J
= 2880 Hz).
P-Pt
9.5.3.8
1,1,1-Tris[4-{
Trans
-Pt(PEt
3
)
2
(NO
3
)}Ethynylphenyl]
Ethane (19)
A solution of 1,1,1-tris[4-(
trans
-Pt(PEt
)
I)ethynylphenyl]ethane
3
2
(28.0 mg, 0.16
mmol) solution in methanol. After stirring for 1 h the yellowish
white AgI was filtered through celite and the solvent was removed to
yield
(110 mg, 0.05 mmol) in CHCl
was added to a AgNO
3
3
19
(90.2 mg) in 90% yield. Anal. calcd. for C
H
N
O
P
Pt
:
62
105
3
9
6
3
1
C, 41.20; H, 5.85; N, 2.32. Found: C, 40.97; H, 5.67; N, 2.21.
H NMR in
(CDCl
, 400 MHz):
δ
7.1 (d, 6H, Ph-H), 6.9 (d, 6H, Ph-H), 2.0 (s, 3H,
3
31
1
CH
), 1.9 (q, 36H, PEt
), 1.2 (t, 54H, PEt
).
P{
H} NMR (CDCl
, 120
3
3
3
3
MHz):
δ
20.1 (s,
1
J
= 3072 Hz). MS (ESI): 1807.5 [M + H]
+
, 1274.7
P-Pt
3
-
+
°
[M - 4PEt
- NO
]
. Melting point: (>270
C, dec.).
3
9.5.3.9
Synthesis of the Prism 17
A solution of
(2.86 mg, 0.009 mmol) in methanol was added
to a stirred solution of
15
(12 mg, 0.01 mmol) in acetone and this
resulting solution was kept under stirring at 50 ºC for 12 h. The
14
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