A kind of phosphine-containing carboxylic acid compound and its preparation method
A compound and phosphine carboxylic acid technology, applied in the field of phosphine-containing carboxylic acid compounds and their preparation, can solve the problems of long synthesis route and harsh reaction conditions, and achieve the effects of mild reaction conditions, overcoming long reaction route and good industrial application prospect.
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Embodiment 1
[0042]A phosphine-containing carboxylic acid compound whose chemical structural formula is:
[0043]
[0044]The reaction equation is:
[0045]
[0046]The preparation method of the compound is as follows:
[0047](1) Add 45mg, 0.2mmol enamide (1a) to a dry 10mL Shrek tube, then transfer the reaction tube to the glove box, then add 49mg, 0.24mmol diphenylphosphine oxide (2a) and 41mg, 0.3 mmol potassium carbonate;
[0048](2) Take out the reaction tube and connect it to the double-row tube connected to the carbon dioxide cylinder. Fill the double-row tube with carbon dioxide 3 times, remove the nitrogen from the tube, and make the tube full of carbon dioxide gas, and then under the carbon dioxide atmosphere Add 2mL DMF and photosensitizer 4CzIPN (32μL, 0.1mol%, 5mg dissolved in 1mL DMF);
[0049](3) Finally, place the reaction solution 2-3cm away from the 30W blue LED light, stir at room temperature (25°C) for 12 hours, then quench the mixture with 4.5mL water and 0.5mL 2N hydrochloric acid, and then us...
Embodiment 2
[0052]A phosphine-containing carboxylic acid compound whose chemical structural formula is:
[0053]
[0054]The reaction equation is:
[0055]
[0056]The preparation method of the compound is:
[0057](1) Add 45mg, 0.2mmol enamide (1a) and 4CzIPN (4mg, 2mol%) to a 10mL dry Shrek tube, then transfer the reaction tube to the glove box, and then add 98mg, 0.3mmol cesium carbonate;
[0058](2) Take out the reaction tube and connect it to the double-row tube connected to the carbon dioxide cylinder. Fill the double-row tube with carbon dioxide 3 times, remove the nitrogen from the tube, and make the tube full of carbon dioxide gas, and then under the carbon dioxide atmosphere Add 2mL DMF and 31μL, 0.24mmol diethyl phosphite (2g);
[0059](3) Finally, place the reaction solution 2-3 cm away from the 30W blue LED light, stir at room temperature (25°C) for 12 hours, then add 5 mL of water, and extract with ethyl acetate for at least 3 times to remove impurities, then 0.5 mL of 2N hydrochloric acid was added, ...
Embodiment 3
[0062]A phosphine-containing carboxylic acid compound whose chemical structural formula is:
[0063]
[0064]The reaction equation is:
[0065]
[0066]The preparation method of the compound is:
[0067](1) Add 1mg, 0.5mol% 4CzIPN to a 10mL dry Shrek tube, then transfer the reaction tube to the glove box and add 49mg, 0.24mmol diphenylphosphine oxide (2a) and 98mg, 0.3mmol cesium carbonate;
[0068](2) Take out the reaction tube and connect it to the double-row tube connected to the carbon dioxide cylinder. Fill the double-row tube with carbon dioxide 3 times, remove the nitrogen from the tube, and make the tube full of carbon dioxide gas, and then under the carbon dioxide atmosphere Add 2mL DMF and 23μL, 0.2mmol styrene (8a);
[0069](3) Finally, place the reaction solution 2-3cm away from the 30W blue LED light, stir at room temperature (25°C) for 12 hours, then quench the mixture with 4.5mL water and 0.5mL 2N hydrochloric acid, and then use ethyl acetate The ester extraction reaction mixture is at le...
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