Heavy-oxygen labeled amide compound synthesized by using thioacid amide, preparation method and application
A technology for labeling amides and thioamides, which can be used in the preparation of peptides, the preparation of organic compounds, and the preparation of carboxylic acid amides, etc., and can solve the problems of a large number of heavy metal wastes, difficult post-processing and purification, and high toxicity.
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Embodiment 1
[0030] A preparation method of a heavy oxygen-labeled amide compound synthesized with thioamide, the synthetic route is as follows:
[0031]
[0032] The specific synthesis method is as follows:
[0033] At room temperature, add 179mg (1mmol) N-benzylthiopropionamide, 101mg triethylamine and 60mg heavy oxygen water into a 20mL round bottom flask equipped with a magnetic stirrer, seal with a rubber stopper, protect it with nitrogen, and then use a syringe Add 10mL of anhydrous acetonitrile into the round bottom flask, then stir at a speed of 200r / min for 1min, then add 178mg (1mmol) of N-bromosuccinimide into the round bottom flask, and stir at a speed of 500r / min speed response;
[0034] During the experiment, silica gel plate thin layer chromatography (TLC) was used to monitor the reaction progress. Since the polarities of the raw materials and products are different on TLC, TLC can be used to monitor the progress of the reaction. The developer used for TLC monitoring is...
Embodiment 2
[0038] A preparation method of a heavy oxygen-labeled amide compound synthesized with thioamide, the synthetic route is as follows:
[0039]
[0040] The specific synthesis method is as follows:
[0041] At room temperature, add 366mg (1mmol) tert-butoxycarbonyl-L-alanthiol-L-phenylalanine, 79mg pyridine and 60mg heavy oxygen water to a 20mL round-bottomed flask equipped with a magnetic stirrer, with a rubber stopper Seal, nitrogen protection, and then add anhydrous ethyl acetate 10mL with a syringe, then stir at a speed of 200r / min for 3min, then add 134mg (1mmol) N-chlorosuccinimide into the reaction vessel, and 500r / min speed;
[0042] During the experiment, TLC was used to monitor the reaction process. When the reaction was monitored to be complete, the reaction was stopped, and then the reaction solution was filtered, concentrated, and purified to obtain 349 mg of white powdered tert-butoxycarbonyl-L-alanyl- 18 O-L-phenylalanine.
[0043] After analysis, the prepare...
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