Gadolinium complex used for solution paramagnetic relaxation enhancement probe and synthetic method thereof
A technology of paramagnetic relaxation enhancement and synthesis method, which can be applied to compounds containing Group 3/13 elements of the periodic table, Group 3/13 organic compounds without C-metal bonds, chemical instruments and methods, etc. , the research on the impact structure, etc., to achieve the effect of simple operation, reduced impact, and simple response
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Embodiment 1
[0025] Add 1 equivalent of DTPAA to 50 equivalents of dry DMF, add 10 equivalents of ethanolamine, the white solid dissolves rapidly, react at room temperature under argon protection for 12 hours, remove the solvent by rotary evaporation, dissolve the obtained solid in deionized water, and adjust the pH value to 4, add 0.5 equivalent of gadolinium oxide, reflux for 24 hours. After concentration, 40 equivalents of ethanol was added to precipitate a white solid. Filter and wash the white solid 5 times with ethanol or acetone. Then it was dissolved in deionized water, passed through a sodium ion exchange resin, the effluent was collected, and the solvent was removed by rotary evaporation to obtain a white powder, that is, Gd-DTPA-BEA. ESI-MS detection, C18H29GdN5010 [M+Na] + calculated value = 657.10 experimental value = 657.13.
Embodiment 2
[0027] Add 1 equivalent of DTPAA to 50 equivalents of dry DMF, add 5 equivalents of ethanolamine, the white solid dissolves rapidly, and react at room temperature under argon protection for 12 hours, remove the solvent by rotary evaporation, dissolve the obtained solid in deionized water, and adjust the pH value to 1, add 0.5 equivalent of gadolinium oxide, reflux for 24 hours. After concentration, 20 equivalents of ethanol was added to precipitate a white solid. Filter and wash the white solid 5 times with ethanol or acetone. Then it was dissolved in deionized water, passed through a sodium ion exchange resin, the effluent was collected, and the solvent was removed by rotary evaporation to obtain a white powder, namely Gd-DTPABEA. ESI-MS detection, C18H29GdN5010 [M+Na] + calculated value = 657.10 experimental value = 657.13.
Embodiment 3
[0029] Add 1 equivalent of DTPAA to 50 equivalents of dry DMF, add 6 equivalents of ethanolamine, the white solid dissolves rapidly, react at room temperature under argon protection for 12 hours, remove the solvent by rotary evaporation, dissolve the obtained solid in deionized water, and adjust the pH value to 2, add 0.5 equivalents of gadolinium oxide, and reflux for 24 hours. After concentration, 25 equivalents of ethanol was added to precipitate a white solid. Filter and wash the white solid 5 times with ethanol or acetone. Then it was dissolved in deionized water, passed through a sodium ion exchange resin, the effluent was collected, and the solvent was removed by rotary evaporation to obtain a white powder, namely Gd-DTPABEA. ESI-MS detection, C18H29GdN5010 [M+Na] + calculated value = 657.10 experimental value = 657.13.
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