Preparation method of tritium labeled diaveridine
A technology of dimethoxybenzidine and dimethoxy, which is applied in the field of radiochemical synthesis, can solve the problems of difficulty in obtaining qualified labeled products, high requirements for test equipment and raw materials, and complicated operations, and achieves easy control, no Leak hazard, clearly marked effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0033](1) Add 5.5 g of sodium methoxide and 40 ml of methanol in sequence in a reaction vessel equipped with a stirring device and equipped with a thermometer 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 was 86%.
[0034] (2) Add sodium methylate 2g, methyl alcohol 20ml successively in the reaction vessel equipped with a thermometer with a stirring device, add guanidine carbonate 3.4g, the α-(methoxymethyl)-3 obtained in the previous step after stirring and dissolving, 2g of 4-...
Embodiment 2
[0036] (1) Add 20 g of sodium methoxide and 100 ml of methanol in sequence in a reaction vessel equipped with a stirring device and equipped with a thermometer 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%.
[0037] (2) Add 9 g of sodium methylate and 60 ml of methanol successively in a reaction vessel with a stirring device equipped with a thermometer. After stirring and dissolving, add 10 g of guanidine carbonate and...
Embodiment 3
[0039] In the 5mL micro-reaction bottle, add magneton successively, then add 5-bromo-dimethoprim prepared in Example 1 50mg, add 3mL methanol to make it completely dissolved, then add 10% concentration of Pd / C 25mg. The reaction bottle was placed on a tritiation device (manufactured by RC TRITEC, Switzerland) and high-purity tritium gas was introduced, the reaction pressure was adjusted to 200 mmHg, and the reaction was kept at 50° C. for 2 h 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.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More