Novel BAPTA derivative, preparation method thereof and medicinal use thereof
A pharmacy, drug technology, applied in the field of improved BAPTA derivatives, which can solve problems affecting R&D and production
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Embodiment 1
[0026] Embodiment 1: the preparation of BAPTA methyl ester
[0027] In a 10L dry reaction kettle, add 370g (1.5mol) of 2,2'-diaminoethylene glycol diphenyl ether and 3500ml of anhydrous acetonitrile, stir at room temperature for 10min, and 2 Under protection, 1440ml (8.32mol) of diisopropylethylamine and 70g (0.446mol) of anhydrous sodium iodide were added, and the temperature was raised slowly. When the temperature of the reaction solution reached 60°C-65°C, 768ml of methyl bromoacetate ( 8.32mol), after the dripping is completed, seal the reactor, raise the temperature to 80℃~83℃, react and stir for 27h, TLC controls the reaction end point, the developer is DMF-ethyl acetate=6:20, the reaction is completed, cooled to At room temperature, add 4000ml of toluene, stir for 10min, separate the toluene layer, continue to stir and separate the solid compound with 1000ml×4 toluene, combine the toluene layer, wash the toluene layer with 1000ml×4 deionized water, discard the water lay...
Embodiment 2
[0034] Embodiment 2: the preparation of BAPTA
[0035]In a 10L clean reaction kettle, add 532g (1.0mol) of BAPTA methyl ester and 5500ml of ethanol, heat slowly until the solids are completely dissolved, and slowly add 2667ml (5.0mol) of 15% sodium hydroxide solution [prepared by 15% sodium hydroxide solution Method: Weigh 400g of sodium hydroxide, dissolve in 2600ml of distilled water, stir to clarify, and cool to obtain], after the dropwise addition, reflux the mixture for 3 hours, TLC to control the reaction end point, the developer is DMF-ethyl acetate=1:2, After the reaction is over, cool slightly, add 15g of activated carbon, stir and reflux for 20min, remove insoluble matter by filtration, concentrate under reduced pressure to leave one-tenth of the solvent, cool to room temperature, add 1L of distilled water, cool to 5°C-10°C, use 0.1N Adjust the pH ester to 2-2.5 with hydrochloric acid, keep stirring for 20 minutes, filter, wash the solid with distilled water until th...
Embodiment 3
[0037] Example 3: Preparation of 1,2-bis(2-aminophenoxy)ethane-N,N,N',N'-tetra(dimethylaminoethanol)tetraacetate
[0038] In a 5000ml dry and clean four-neck flask, add BAPTA95g (0.2mol), anhydrous acetonitrile 1100ml, stir at room temperature for 10min, and 2 Under protection, add 208ml (1.2mol) of diisopropylethylamine and 12g (0.08mol) of anhydrous sodium iodide, and slowly raise the temperature. When the temperature of the reaction solution reaches 60℃~65℃, slowly drop in dimethylaminoethyl Bromine 216g (1.2mol) [Dimethylaminoethyl bromide preparation method: Take 500g of commercially available dimethylaminoethyl bromide hydrobromide, dissolve it in 1500ml distilled water, adjust the pH to 9 with saturated sodium bicarbonate solution , extracted with 3000ml of toluene, dried over anhydrous sodium sulfate, filtered, and concentrated to dryness], after the dropwise addition, seal the reactor, raise the temperature to 80°C to 83°C, stir the reaction for 30h, and control the e...
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