Complex with amide-amine as side chain and its preparation method and application
A complex and amide technology, which is applied in the preparation of carboxylic acid amides, organic compounds, preparations for in vivo tests, etc., can solve the problems of low toxicity and side effects, low relaxation efficiency, etc., and achieve the effect of low toxicity
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[0046] The preparation method of the complex with amide-amine as the side chain of the present invention, the steps are as follows:
[0047] Step 1, the synthesis of 1,4-bis(4-oxobutyrate ethyl)benzene
[0048] Dissolve the compound and the base in a ketone solvent, add iodide and ethyl 4-bromobutyrate to obtain a mixed solution A, reflux the mixed solution A at 65-75°C overnight, then stop the reaction, distill off the solvent under reduced pressure, and Add absolute ethanol to the remaining reaction solution, heat and reflux at 65°C to 75°C for 5 to 10 minutes, put it in an ice-water bath to cool, and obtain a light brown solid, which is 1,4-bis(4-oxobutyrate ethyl)benzene;
[0049] Wherein, the compound is shown in formula III or formula IV:
[0050]
[0051] In formula III and formula IV, R 1 , R 2 , R 3 , R 4 All are substituents, the same or different, respectively hydroxyl, amino, carboxyl or alkyl;
[0052] The base is potassium carbonate, sodium carbonate, ce...
Embodiment 1
[0072] The synthesis of embodiment 1 Gd-DBAM
[0073] Step 1, the synthesis of 1,4-bis(4-oxobutyrate ethyl)benzene
[0074] Dissolve 1.1g of hydroquinone and 7.5g of potassium carbonate in 50ml of acetone, add 0.83g of potassium iodide and 4.5ml of ethyl 4-bromobutyrate to obtain a mixed solution A, and reflux the mixed solution A at 65°C overnight to stop the reaction , the solvent acetone was distilled off under reduced pressure, 6ml of absolute ethanol was added to the remaining reaction solution, heated to reflux at 90°C for 10min, cooled and crystallized in an ice-water bath for 30min, filtered under reduced pressure, rinsed with deionized water at 0°C, and dried to obtain shallow 1.34 g of brown solid 1,4-bis(4-oxobutyrate ethyl)benzene.
[0075] Step two, aminolysis reaction
[0076] Mix 30ml of ethylenediamine and 75ml of absolute ethanol evenly to obtain a mixed solution B, add 1.014g of 1,4-bis(4-oxobutyrate ethyl)benzene obtained in step 1 into the mixed solution ...
Embodiment 2
[0083] The synthesis of embodiment 2 Gd-DBAM
[0084] Step 1, the synthesis of 1,3-two (4-oxobutyrate ethyl) benzene
[0085] Dissolve 4.4g of resorcinol and 3.32g of potassium iodide in 200ml of acetone, add 30g of potassium carbonate and 18ml of ethyl 4-bromobutyrate to obtain a mixed solution A, and reflux the mixed solution A at 65°C overnight to stop the reaction and reduce Remove the solvent acetone by pressure distillation, add 24ml of absolute ethanol to the remaining reaction solution, heat and reflux at 90°C for 10min, put it in an ice-water bath to cool and crystallize for 30min, filter under reduced pressure, rinse with deionized water at 0°C, and dry to obtain a light brown solid 12.56 g of 1,4-bis(4-oxobutyrate ethyl)benzene.
[0086] Step two, aminolysis reaction
[0087]Mix 47.3ml of ethylenediamine and 118ml of absolute ethanol evenly to obtain a mixed solution B, add 1.599g of 1,3-bis(4-oxobutyrate)benzene obtained in step 1 into the mixed solution B, and r...
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