Two methods of preparation of the organometallic precursor[188Re(CO)3(H2O)3]+ in aqueous were present in this paper.One method uses gaseous carbon monoxide and amine borane(BH3·NH3) as the reducing agent.In other...Two methods of preparation of the organometallic precursor[188Re(CO)3(H2O)3]+ in aqueous were present in this paper.One method uses gaseous carbon monoxide and amine borane(BH3·NH3) as the reducing agent.In other method,CO(g) is replaced by K2[H3BCO2]that releases carbon monoxide during hydrolysis.Both procedures were prepared as radiolabled kits,affording the desired precursor in yields 85% after 20 min at 75 °C.The routine kit-preparation of the precursor[188Re(CO)3(H2O)3]+ in combination with tailor-made ligand systems enables the organometallic labeling of biomolecules with unprecedented high specific activities.展开更多
In order to study the effects of the substituted groups on the properties of the complexes, a series of rhenium(Ⅰ) 2,2′-bipyridyl complexes [fac-(4,4′-di-COOEt-bpy)Re(CO) 3(X—pyridine)PF 6], where bpy is 2,2′-bip...In order to study the effects of the substituted groups on the properties of the complexes, a series of rhenium(Ⅰ) 2,2′-bipyridyl complexes [fac-(4,4′-di-COOEt-bpy)Re(CO) 3(X—pyridine)PF 6], where bpy is 2,2′-bipyridine and X is 4-methyl, 3-hydroxy, 4-hydroxy, 4-amino, or H, were synthesized with a yield more than 90%, and characterized by 1H NMR, 13C NMR, 2D-NMR( 1H- 1H COSY, HMBC, HSQC), ESI-MS and HRMS. The δ H values on the X—pyridine ring were shifted to up-field in 1H NMR and the MLCT absorbance maxima were red-shifted as the X groups became more electron-donating from H to 4-methyl, 4-hydroxy or 4-amino. The ESI-MS and HRMS showed the mono-charged peaks and their isotopic peaks of the complexes. The absorption maximum of 1d(X= 4-amino) is 20 nm longer than that of 1e(X=H). It might be used to broaden the absorption range of solar cells.展开更多
Click chemistry was used to study on radiolabeling of 1,2,3-triazole analogs with fac-[188 Re(CO) 3 (H 2 O) 3]+ . CuSO 4 /L-sodium ascorbate was chosen as the catalyst system, three terminal alkynes were conjugated wi...Click chemistry was used to study on radiolabeling of 1,2,3-triazole analogs with fac-[188 Re(CO) 3 (H 2 O) 3]+ . CuSO 4 /L-sodium ascorbate was chosen as the catalyst system, three terminal alkynes were conjugated with two different azides respectively, and then the new prepared fac-[188 Re(CO) 3 (H 2 O) 3]+ was coordinated to the six triazoles. The results showed that the radiochemical yields (RCY) of the conjugation of fac-[188 Re(CO) 3]+ with six triazoles were over 90%, and the triazoles showed high stability in phosphate-buffered saline and new-born calf serum. The preliminary biological evaluation results showed that the new 188 Re-labeling method via click chemistry could have general application in labeling bioactive molecules in high radiochemical yield and high specific activity for further SPECT research.展开更多
文摘Two methods of preparation of the organometallic precursor[188Re(CO)3(H2O)3]+ in aqueous were present in this paper.One method uses gaseous carbon monoxide and amine borane(BH3·NH3) as the reducing agent.In other method,CO(g) is replaced by K2[H3BCO2]that releases carbon monoxide during hydrolysis.Both procedures were prepared as radiolabled kits,affording the desired precursor in yields 85% after 20 min at 75 °C.The routine kit-preparation of the precursor[188Re(CO)3(H2O)3]+ in combination with tailor-made ligand systems enables the organometallic labeling of biomolecules with unprecedented high specific activities.
文摘In order to study the effects of the substituted groups on the properties of the complexes, a series of rhenium(Ⅰ) 2,2′-bipyridyl complexes [fac-(4,4′-di-COOEt-bpy)Re(CO) 3(X—pyridine)PF 6], where bpy is 2,2′-bipyridine and X is 4-methyl, 3-hydroxy, 4-hydroxy, 4-amino, or H, were synthesized with a yield more than 90%, and characterized by 1H NMR, 13C NMR, 2D-NMR( 1H- 1H COSY, HMBC, HSQC), ESI-MS and HRMS. The δ H values on the X—pyridine ring were shifted to up-field in 1H NMR and the MLCT absorbance maxima were red-shifted as the X groups became more electron-donating from H to 4-methyl, 4-hydroxy or 4-amino. The ESI-MS and HRMS showed the mono-charged peaks and their isotopic peaks of the complexes. The absorption maximum of 1d(X= 4-amino) is 20 nm longer than that of 1e(X=H). It might be used to broaden the absorption range of solar cells.
基金Supported by National Natural Science Foundation of China(No.10875163)Natural Science Foundation of Guangdong Province(Nos.2009B030108036 and S2012010010685)
文摘Click chemistry was used to study on radiolabeling of 1,2,3-triazole analogs with fac-[188 Re(CO) 3 (H 2 O) 3]+ . CuSO 4 /L-sodium ascorbate was chosen as the catalyst system, three terminal alkynes were conjugated with two different azides respectively, and then the new prepared fac-[188 Re(CO) 3 (H 2 O) 3]+ was coordinated to the six triazoles. The results showed that the radiochemical yields (RCY) of the conjugation of fac-[188 Re(CO) 3]+ with six triazoles were over 90%, and the triazoles showed high stability in phosphate-buffered saline and new-born calf serum. The preliminary biological evaluation results showed that the new 188 Re-labeling method via click chemistry could have general application in labeling bioactive molecules in high radiochemical yield and high specific activity for further SPECT research.
