Technetium-and rhenium-bis(heteroaryl) complexes, and methods of use thereof
A technology of heteroaryl and aryl, applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, pharmaceutical formulations, etc. Problems with different structures, weak ability to retain marks, etc.
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[0060] 4. Preparation and characterization of Tc and Re fluorescent SAAC
[0061] Recently we reported the synthesis of a single amino acid chelate (SAAC) Tc(I) binding ligand (1, Figure 4). As shown in this article, SAAC can be combined with {M(CO) 3 } +1 The core forms an inert complex (M=Re, 99m Tc) and can be introduced into the polypeptide if it is a neutral amino acid. In order to prepare its Re complex to be fluorescent while maintaining the binding 99m Tc-capable SAAC-type ligand, in Na(OAc) 3 In the presence of BH, N-α-9-fluorenylmethoxycarbonyl-L-lysine is reacted with isoquinolinal to obtain bifunctional ligand 3 (Figure 4). The desired product can be prepared in the order of grams, and the desired product can be separated with excellent yield after column chromatography. By making ligand 3 and [NEt 4 ] 2 [Re(CO) 3 Br 3 ] Reaction to synthesize Re complex 4a. The TEA salt form of the complex is separated by column chromatography.
[0062] Figure 5a shows the absorption ...
Embodiment 1
[0427] 1. Synthesis of N-α-(tert-butoxycarbonyl)-N-ω-bis(2-pyridylmethyl)-L-lysine (L1c-Boc)
[0428] 2-Chloromethylpyridine hydrochloride (1.4g, 8.53mmol) and N-α-(tert-butoxycarbonyl)-L-lysine (1g, 4.06mmol) were dissolved in water and stirred at room temperature Five days, add 5mol dm at intervals-3 Aqueous NaOH keeps the pH at 8-10. The dark red solution was extracted with ethyl acetate, followed by 1mol dm -3 HCl acidified the aqueous phase to a pH of 3-4, extracted with chloroform and concentrated. The residue was purified by column chromatography using 10% chloroform in methanol to obtain N-α-(tert-butoxycarbonyl)-N-ω-bis(2-pyridylmethyl)-L-lysine (950mg, 55 %). 1 HNMR(CDCl 3 ), 300 MHz): 1.41 (s, 9H), 1.26-1.62 (m, 6H), 2.58 (t, 2H), 3.84 (s, 4H), 4.24 (t, H), 7.15 (m, 2H), 7.48 (d, 2H), 7.65 (m, 2H), 8.53 (d, 2H). 13 C NMR(CD 3 OD, 300MHz): 24.31 (C, CH 2 ), 26.66 (C, CH 2 ), 28.93 (3C, t-Bu), 33.15 (C, CH 2 ), 55.50(C, NCH 2 ), 60.12(2C, PyCH 2 ), 80.06 (C, NCH) 124.34 (...
Embodiment 2
[0430] 1. Synthesis of N-α-(2-pyridylmethyl)-N-ω-(tert-butoxycarbonyl)-L-lysine (L2d-Boc)
[0431] 2-Chloromethylpyridine hydrochloride (730mg, 4.46mmol) and N-α-(tert-butoxycarbonyl)-L-lysine (1g, 4.06mmol) were dissolved in water and stirred at room temperature for two Add 5mol dm every day -3 Aqueous NaOH keeps the pH at 8-10. The dark red solution was extracted with ethyl acetate, followed by 1mol dm -3 HCl acidified the aqueous phase to pH 6, then treated with chloroform, the desired product precipitated out, the precipitate was filtered and dried under vacuum (670 mg, 49%).
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