A complex of a bifunctional linker coordinated with a metal carbonyl core and a preparation method thereof
A bifunctional linker, metal carbonyl technology, applied to 7/17 groups of organic compounds without C-metal bonds, preparations for in vivo experiments, and isotope introduction of organic compounds, etc. suitability etc.
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Embodiment 1
[0074] 99m Tc(CO) 3 -L 2 Preparation of complexes:
[0075] (1) Ligand L 2 Synthesis
[0076] Synthesis of compound 3 (3-(4-hydroxyphenyl)propionic acid methyl ester): p-hydroxyphenylpropionic acid (3g, 18.1mmol) and 50mL of methanol were added to the round-bottomed flask, and then trifluoroethylene was added dropwise to the mixed solution Boronium diethyl ether (0.3mL) was stirred at room temperature for 6 hours, and the organic phase in the filtrate was removed under reduced pressure using a rotary evaporator, and separated by a silica gel column with n-hexane / ethyl acetate (v / v, 2 / 8). Collect target component, remove solvent under reduced pressure, obtain 2.72g white solid (yield: 84%);
[0077] 1 HNMR (400MHz, CDCl 3 )δ: 7.07(d, 2H, J=8.4Hz), 6.76(d, 2H, J=8.4Hz), 4.72(s, 1H), 3.68(s, 3H), 2.89(t, 2H, J=7.6 Hz), 2.60 (t, 2H, J=7.6Hz); HRMS (ESI) theoretical molecular weight C 10 h 13 o 3 (M+H) + , 181.0865; measured molecular weight, 181.0815;
[0078] Synthes...
Embodiment 2
[0098] 99m Tc(CO) 3 -L 3 Preparation of complexes:
[0099](1) Ligand L 3 preparation of
[0100] 1) Double activated (HBED-CC) TFP 2 Synthesis:
[0101] From compound 1 (N, N'-bis[2-hydroxyl-5-(carboxyethyl) benzyl]ethylenediamine-N, N'-diacetic acid) as the reaction starting material, compound 1 and ferric chloride Mix and stir at room temperature for 20 minutes according to the equivalent of 1:1.1, and the product is purified by flash chromatography to obtain [Fe(HBEDCC)] – ; to 1000 μL concentration of 0.01M [Fe(HBED-CC)] – Add 10 equivalents of TFP (trifluopyrazine) and 4 equivalents of N, N'-diisopropylcarbodiimide to the DMF solution of DMF, react at room temperature for 3 days, and purify the product by preparative HPLC to obtain [ Fe(HBED-CC)]TFP 2 , after diluting with water, the diluted [Fe(HBED-CC)]TFP 2 The solution was injected onto the RP18 column, and the RP18 filter column was washed with 3mL, 1M hydrochloric acid and washed with 4mL of H 2 O washin...
Embodiment 3
[0115] Re(CO) 3 -L 2 Preparation of complexes
[0116] An aqueous solution of 10ml rhenium pentacarbonyl bromide (80mg, 0.2mmol) was refluxed at 105°C for 24 hours, and then the L 2 (30mg, 0.038mmol) added to containing Re (CO) 3 (H 2 O) 3 In the above reaction solution (2 mL) of the Br intermediate, the mixture was acidified with 0.1 N HCl to pH = 5 and heated at 95 °C for 3 h to give Re(CO) 3 -L 2 complex; its possible structure is as follows, such as image 3 Shown, is the Re(CO) prepared by Example 3 of the present invention 3 -L 2 UV-LC analysis chart. The analysis results show that the product has only one structure, and the existence of split peaks indicates that there are chiral isomers in the structure of the complex.
[0117]
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