High-specific-activity tritium-labeled sulfamethoxazole and preparation method thereof
A technology of sulfamethoxazole and methylisoxazole, applied in organic chemical methods, antibacterial drugs, active ingredients of heterocyclic compounds, etc., can solve problems such as limited resources, high price of radioisotope sources, and unstable labeling sites, etc. problems, to achieve the effect of low preparation cost, high chemical purity and high yield
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[0057] Such as figure 1 As shown, the method for preparing tritium-labeled sulfamethoxazole with high specific activity provided in the embodiment of the present invention includes:
[0058] S101, dissolve m-bromoaniline and triethylamine in dichloromethane, and add equimolar trifluoroacetic anhydride dropwise at 0-5°C. After the dropwise addition is completed, the temperature is raised to room temperature and the reaction is stirred for 2 to 4 hours. The reaction solution is washed with saturated sodium chloride, the dichloromethane layer is dried with anhydrous sodium sulfate, filtered, and the solvent is evaporated under reduced pressure to obtain crude trifluoride in white powder. Acetyl meta-bromoaniline.
[0059] S102, take the trifluoroacetyl meta-bromoaniline prepared in step S101 and place it in a round bottom flask, add 0.1-0.5 times the amount of anhydrous sodium sulfate, keep the temperature at 0-5°C, slowly add chlorosulfonic acid and chlorination aid Thionyl chlorid...
Embodiment 1
[0071] (1) Dissolve 7.23g (0.04mol) of meta-bromoaniline and 6.7mL (0.05mol) of triethylamine in 100mL of dichloromethane, and add 8.4g of trifluoroacetic anhydride (0.04mol) dropwise at 0°C. After the dropwise addition, the reaction solution was raised to room temperature and stirred for 3 hours. The reaction solution was washed with saturated sodium chloride, the dichloromethane layer was dried with anhydrous sodium sulfate, filtered, and the solvent was evaporated under reduced pressure to obtain crude trifluoroacetyl as a white powder. M-Bromoaniline, the yield is 78%.
[0072] (2) Take 4.0g (0.015mol) of trifluoroacetyl meta-bromoaniline prepared in step (1) and place it in a 50mL round-bottomed flask, add 2.1g (0.015mol) of anhydrous sodium sulfate as an auxiliary, and place it in an ice bath After cooling to 0°C, slowly add 1 mL (0.015 mol) of chlorosulfonic acid and 0.55 mL (0.0075 mol) of thionyl chloride as a chlorination assistant. After the addition, the reaction solu...
Embodiment 2
[0077] (1) Dissolve 7.23g (0.04mol) of meta-bromoaniline and 6.7mL (0.05mol) of triethylamine in 100mL of dichloromethane, and add 10.6g of trifluoroacetic anhydride (0.05mol) dropwise at 0°C. After the addition is complete, the temperature is raised to room temperature and the reaction is stirred for 3 hours. The reaction solution is washed with saturated sodium chloride, the dichloromethane layer is dried over anhydrous sodium sulfate, filtered, and the solvent is evaporated under reduced pressure to obtain crude trifluoroacetyl as a white powder. The yield of m-bromoaniline was 93.9%.
[0078] (2) Take 4.0g (0.015mol) of trifluoroacetyl meta-bromoaniline prepared in step (1) and place it in a 50mL round-bottomed flask, add 4.3g (0.03mol) of anhydrous sodium sulfate as an auxiliary, and place it in an ice bath After cooling to 0°C, slowly add 2 mL (0.03 mol) of chlorosulfonic acid and 0.55 mL (0.0075 mol) of thionyl chloride as a chlorination assistant. After the addition is co...
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