Example 10
Re(bpy)(CO)3(OCOH) (Sometimes Abbreviated as Re—OCOH)
An ethanol/water mixed solution (1:1 v/v, 50 mL) containing Re(bpy)(CO)3Br (301 mg, 5.95×10−1 mmol) and an excessive amount of sodium formate (4.05 g, 59.6 mmol) was heated to reflux overnight. The ethanol was slowly distilled off under reduced pressure. Dichloromethane was added thereto, and the resultant was extracted with water three times. After distilling off the solvent of the thus obtained organic layer under reduced pressure, the resultant was recrystallized from acetone/diethyl ether/hexane, and a yellow solid thus obtained was dried under reduced pressure.
Yield: 70.4 mg (1.49×10−1 mmol), Yield: 25.1%
ESI-MS in MeCN m/z=626 [M-PF6+]+
FT-IR in CH2Cl2 ν(CO)/cm−1: 2022, 1918, 1896
1H-NMR in CD3CN (298 MHz): δ (ppm)=9.02 (dd, 2H, J=5.6, 1.6 Hz, bpy-6,6′), 8.40 (dd, 2H, J=8.3, 1.1 Hz, bpy-3,3′), 8.20 (ddd, 2H, J=8.3, 8.3, 1.6 Hz, bpy-4,4′), 7.61 (ddd, 2H, J=8.3, 5.6, 1.1 Hz, bpy-5,5′), 7.81 (s, 1H, HCOO)
Elemental analysis: Calcd. (%) for C14H9N2O5Re: C, 35.67; H, 1.92; N, 5.94.
Found: C, 35.63; H, 1.82; N, 6.01
