Palladium(II) Complexes
1051
Fig. 1. The synthesis routes of the six Pd(II) complexes.
68%. IR (KBr, cm¡1): n(Amide&)1551, n(OCO)a 1632, n(OCO)a NbzpheH2 (37.71 mg, 0.12 mmol). Yield: 62%, yellow solid.
1383, n(Pd-N) 566, n(Pd-O) 465. 1H NMR (600 MHz, d6- IR (KBr, cm¡1): n(OH) 3428, n(Amide&) 1552, n(OCO)a 1640,
1
DMSO) d (ppm): 3.08 (dd, J D 13.1, 4.5 Hz, 1H, CH2-H), n(OCO)a 1397, n(Pd-N) 565, n(Pd-O) 479. H NMR (600 MHz,
3.29 (dd, J D 13.1, 4.5 Hz, 1H, CH2-H), 5.08–5.05 (m, 1H, CDCl3) d (ppm): 3.11 (dd, J D 12.9, 5.7 Hz, 1H, CH2-H),
CH), 6.65 (t, J D 7.5 Hz, 1H, Ar-H), 6.73 (t, J D 7.5 Hz, 2H, 3.44 (dd, J D 12.9, 5.7 Hz, 1H, CH2-H), 5.12–5.06 (m, 1H,
Ar-H), 7.09 (d, J D 3.0 Hz, 3H, Ar-H), 7.13 (d, J D 5.4 Hz, CH-H), 7.19–7.13 (m, 2H, Ar-H), 7.27 (d, J D 7.2 Hz, 2H,
1H, Ar-H), 7.23 (d, J D 7.2 Hz, 2H, Ar-H), 7.28 (d, J D Ar-H), 7.31 (d, J D 5.4 Hz, 1H, Ar-H), 7.81–7.74 (m, 2H,
5.4 Hz, 1H, Ar-H), 7.78–7.75 (m, 1H, Ar-H), 8.02 (t, J D Ar-H), 7.95 (d, J D 9.0 Hz, 2H, Ar-H), 8.03 (t, J D 8.1 Hz,
7.8 Hz, 1H, Ar-H), 8.26 (d, J D 7.8 Hz, 1H, Ar-H), 8.30 (t, J 1H, Ar-H), 8.35–8.26 (m, 4H, Ar-H), 8.43 (d, J D 8.4 Hz,
D 6.9 Hz, 4H, Ar-H), 8.42 (d, J D 7.8 Hz, 1H, Ar-H). ESI- 1H, Ar-H), 8.52 (d, J D 8.4 Hz, 2H, Ar-H). ESI-MS: 592.05
MS: 568.03 [MCK]C. Anal. Calcd. for [Pd(bipy)(Bzphe-N, [M]C. Anal. Calcd. for [Pd(bipy)(p-Nbzphe-N, O)]¢H2O
O)] (C26H21N3O3Pd, 529.06): C, 58.93; H, 3.99; N, 7.93. (C26H22N4O6Pd, 592.06): C, 52.67; H, 3.74; N, 9.45. Found:
Found: C, 58.84; H, 4.04; N, 7.84.
C, 52.75; H, 3.89; N, 9.29.
[Pd(bipy)(p-Mbzphe-N, O)]¢2H2O (I-b)
[Pd(phen)(Bzphe-N, O)]¢2H2O (P-a)
The synthesis of I-b was carried out in an identical manner to The synthesis of P-a was carried out in an identical manner
I-a starting from [Pd(bipy)Cl2] (20 mg, 0.06 mmol) and p- to I-a starting from [Pd(phen)Cl2] (20 mg, 0.056 mmol) and
MbzpheH2 (34.00 mg, 0.12 mmol). Yellow solid, yield: 62%. BzpheH2 (30.16 mg, 0.112 mmol). Yield: 66%, yellow crys-
IR (KBr, cm¡1): n(OH) 3430, n(Amide&) 1530, n(OCO)a 1641, talline. IR (KBr, cm¡1): n(OH) 3428, n(Amide&) 1549, n(OCO)a
1
n(OCO)a 1385, n(Pd-N) 572, n(Pd-O) 455. H NMR (600 MHz, 1637, n(OCO)a 1384, n(Pd-N) 562, n(Pd-O) 474. 1H NMR
CDCl3) d (ppm): 2.07 (s, 3H, CH3), 3.07 (dd, J D 14.1, (600 MHz, CDCl3) d (ppm): 3.14 (dd, J D 14.1, 5.7 Hz, 1H,
5.7 Hz, 1 H, CH2-H), 3.09 (dd, J D 14.1, 5.7 Hz, 1H, CH2- CH2-H), 3.31 (dd, J D 14.1, 5.7 Hz, 1H, CH2-H), 5.13–5.08
H), 5.05–5.02 (m, 1H, CH), 6.65 (t, J D 7.2 Hz, 1H, Ar-H), (m, 1H, CH), 6.26 (d, J D 7.2 Hz, 1H, Ar-H), 6.52 (t, J D
6.72 (t, J D 7.2 Hz, 2H, Ar-H), 6.89 (d, J D 7.8 Hz, 3H, Ar- 7.4 Hz, 2H, Ar-H), 7.07 (d, J D 4.8 Hz, 3H, Ar-H), 7.23 (d, J
H), 7.15–7.11 (m, 1H, Ar-H), 7.22 (d, J D 7.2 Hz, 3H, D 7.2 Hz, 2H, Ar-H), 7.50 (s, 1H, Ar-H), 8.08 (dd, J D 7.8,
Ar-H), 7.27 (d, J D 4.8 Hz, 1H, Ar-H), 7.78–7.74 (m, 1H, 5.2 Hz, 1H, Ar-H), 8.13 (d, J D 8.8 Hz, 1H, Ar-H), 8.20 (d, J
Ar-H), 8.04 (t, J D 7.5 Hz, 1H, Ar-H), 8.21 (d, J D 7.8 Hz, D 8.8 Hz, 1H, Ar-H), 8.39 (m, 2H, Ar-H), 8.65 (dd, J D 12.8,
2H, Ar-H), 8.26 (d, J D 7.8 Hz, 1H, Ar-H), 8.41 (d, J D 5.2 Hz, 2H, Ar-H), 8.91 (d, J D 8.0 Hz, 1H, Ar-H). ESI-MS:
8.4 Hz, 1H, Ar-H). ESI-MS: 580.11 [MCH]C. Anal. Calcd. [MCH]C 590.10. Anal. Calcd. for [Pd(phen)(Bzphe-N, O)]¢
for
[Pd(bpy)(p-Mbzphe-N,O)]¢2H2O
(C27H27N3O5Pd, 2H2O (C28H25N3O5Pd, 589.08): C, 57.01; H, 4.27; N, 7.12.
579.10): C, 55.92; H, 4.69; N, 7.25. Found: C, 56.91; H, 4.68; Found: C, 57.11; H, 4.17; N,7.05.
N, 7.25.
[Pd(en)(Bzphe-N, O)]¢H2O (S-a)
The synthesis of S-a was carried out in an identical manner
[Pd(bipy)(p-Nbzphe-N, O)]¢H2O (I-c)
The synthesis of I-c was carried out in an identical manner to to I-a starting from [Pd(en)Cl2] (20 mg, 0.084 mmol) and
I-a starting from [Pd(bipy)Cl2] (20 mg, 0.06 mmol) and p- BzpheH2 (45.24 mg, 0.168 mmol). Yield: 66%, yellow