The preparation method of tritium-labeled ditrimethoprim
A technology of dimethoprim and dimethoxy, which is applied in the field of radioactive chemical synthesis, can solve the problems of difficulty in obtaining qualified labeled products, high requirements for test equipment and raw materials, and complicated operations, and achieve easy control and radioactivity High chemical purity and high chemical purity, well-defined marker positions
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Embodiment 1
[0029] (1) Add 5.5g of sodium methoxide and 40ml of methanol successively into a reaction vessel with a stirring device to dissolve them. 6.6 mL of acrylonitrile was added dropwise with a constant pressure dropping funnel at 25°C, and reacted for 1 h. Add 5g of 3,4-dimethoxy-5-bromo-benzaldehyde, and react at 50°C for 6h. Add an equal volume of water to the reaction system, remove methanol by distillation under reduced pressure, extract with toluene, dry over anhydrous magnesium sulfate or anhydrous sodium sulfate, filter, and distill under reduced pressure to obtain a yellow oily product α-(methoxymethyl) 5.5 g of -3,4-dimethoxy-5-bromo-cinnamonitrile, the yield is 86%.
[0030] (2) Add 2g of sodium methoxide and 20ml of methanol in turn into a reaction vessel with a stirring device, stir and dissolve, add 3.4g of guanidine carbonate, α-(methoxymethyl)-3,4-dimethyl Oxy-5-bromo-cinnamonitrile 2g, reflux reaction for 4h, after cooling at room temperature, pour the reaction li...
Embodiment 2
[0032](1) Add 20 g of sodium methoxide and 100 ml of methanol in sequence to a reaction vessel with a stirring device to dissolve them. Add 8 mL of acrylonitrile dropwise with a constant pressure dropping funnel at 25°C, and react for 1 h; add 10 g of 3,4-dimethoxy-5-bromo-benzaldehyde, and react for 8 at 50°C; add an equal volume of water to the reaction system, Methanol was distilled off under reduced pressure, extracted three times with ethyl acetate, the ethyl acetate layers were combined, dried over anhydrous sodium sulfate and filtered, the filtrate was distilled off the solvent under reduced pressure to obtain a yellow oily product α-(methoxymethyl)-3 , 11.2 g of 4-dimethoxy-5-bromo-cinnamonitrile, the yield was 88%.
[0033] (2) Add 9g of sodium methoxide and 60ml of methanol in turn into a reaction vessel with a stirring device, stir and dissolve, add 10g of guanidine carbonate, α-(methoxymethyl)-3,4-dimethoxy obtained in the previous step Base-5-bromo-cinnamonitrile...
Embodiment 3
[0035] Into a 5mL micro-reaction vial, add magnetons in sequence, then add 50 mg of 5-bromo-dimethoprim prepared above, add 3 mL of methanol to dissolve it completely, and then add 25 mg of 10% Pd / C. The reaction bottle was placed on a tritiation device (manufactured by RCTRITEC, Switzerland) and high-purity tritium gas was introduced, the reaction pressure was adjusted to 200mmHg, and the reaction was kept at 50°C for 2h with stirring. Stop the reaction, freeze with liquid nitrogen, recover the remaining tritium gas, thaw at room temperature, remove Pd / C by centrifugation, and evaporate the remaining liquid to dryness under reduced pressure to obtain tritium-labeled trimethoprim.
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