An active oxygen-responsive antioxidant nitric oxide donor, its preparation and application
A nitric oxide and antioxidant technology, applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, antidote, etc. Overcome the problem of single function, long half-life and good stability
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Embodiment 1
[0043]Dissolve 15g of 4-hydroxymethylphenylboronic acid pinacol ester (PBAP) in 100mL of chloroform, add 6g of 2-nitrocarbonylimidazole (CDI), stir at 25°C for 2 hours, extract the product with water, and wash with anhydrous sodium sulfate After drying and filtering, the filtrate was rotary evaporated under reduced pressure to obtain 4-nitrocarbonylimidazolylphenylboronic acid pinacol ester (PBAP-CDI), with a yield of >95% and a purity of >98%.
[0044] Dissolve 5g of PBAP-CDI in 25mL of dichloromethane, add 8.5g of 5-monoisosorbide nitro (ISN) and 3.2g of 4-dimethylaminopyridine (DMAP), and stir at 20°C for 72 hours, the product After extracting with water and drying with phosphorus pentoxide, the filtrate was rotary evaporated under reduced pressure, and dried in a vacuum oven to obtain 4-nitrocarbonyl-(5-mononitroisosorbide)-phenylboronic acid pinacol ester ( PBAP-ISN), yield>85%, purity>98%.
[0045] The proton nuclear magnetic resonance spectra of the obtained PBAP-CDI a...
Embodiment 2
[0047] Dissolve 500g of 4-hydroxymethylphenylboronic acid pinacol ester (PBAP) in 1000mL of toluene, add 250g of 2-nitrocarbonylimidazole (CDI), stir at 0°C for 48 hours, extract the product with water, and use anhydrous magnesium sulfate After drying and filtering, the filtrate was rotary evaporated under reduced pressure to obtain 4-nitrocarbonylimidazolylphenylboronic acid pinacol ester (PBAP-CDI), with a yield of >95% and a purity of >98%.
[0048] Dissolve 200g of PBAP-CDI in 200mL of dioxane, add 300g of 5-monoisosorbide nitrate (ISN) and 72g of pyridine, stir at 75°C for 2 hours, extract the product with water, and carry out anhydrous magnesium sulfate After drying, the filtrate was rotary evaporated under reduced pressure, and dried in a vacuum oven to obtain 4-nitrocarbonyl-(5-mononitroisosorbide)-phenylboronic acid pinacol ester (PBAP-ISN) yield 90%.
Embodiment 3
[0050] Dissolve 5g of 4-hydroxymethylphenylboronic acid pinacol ester (PBAP) in 50mL of dimethyl sulfoxide, add 10g of 2-nitrocarbonylimidazole (CDI), stir at 60°C for 24 hours, extract the product with water, and use Phosphorus pentoxide was dried and filtered, and the filtrate was rotary evaporated under reduced pressure to obtain 4-nitrocarbonylimidazolylphenylboronic acid pinacol ester (PBAP-CDI). Yield98%
[0051] Dissolve 2g of PBAP-CDI in 10mL of anisole, add 3g of 5-monoisosorbide (ISN) and 5.7g of 4-dimethylaminopyridine (DMAP), stir at 90°C for 24 hours, and extract the product with water , and after drying with anhydrous sodium sulfate, the filtrate was rotary evaporated under reduced pressure, and dried in a vacuum oven to obtain 4-nitrocarbonyl-(5-mononitroisosorbide)-phenylboronic acid pinacol ester (PBAP- ISN), yield>95%, purity>98%.
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