A compound for ischemia-reperfusion injury and its preparation method
A technology of ischemia-reperfusion and compounds, applied in the field of medicinal chemistry
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Embodiment 1
[0069] Embodiment 1. Preparation of compound 3
[0070]
[0071] Compound 1 (50g, 332.89mmol, 1eq) was dissolved in 500mL of anhydrous tetrahydrofuran, then pyridine (52.92g, 669.03mmol, 54mL, 2.01eq) and 4-dimethylaminopyridine (814mg, 6.66mmol, 0.02eq) were added, Then 4-nitrobenzenesulfonyl chloride (89g, 401.59mmol, 1.21eq) was slowly added at 0°C, and the resulting mixture was stirred at 25°C for 6 hours. LC-MS (EW9132-1-P1A) showed that the main peak was the target signal peak, the reaction solution was filtered, the filter cake was slurried in 300mL of ethyl acetate, and the resulting solid was dried to obtain compound 3 (100g, 255.25mmol, 76.68%yield, 85.6%purity) of a yellow solid, which was analyzed by LC-MS ( EW9132-1-P1B) and NMR (EW9132-1-PA) characterization.
Embodiment 2
[0072] Embodiment 2. Preparation of compound 4
[0073]
[0074] Compound 3 (5.00g, 14.91mmol, 1.00eq), zinc powder (4.00g, 61.17mmol, 4.10eq) and glacial acetic acid (3.68g, 61.20mmol, 4.10eq) were added to 75mL of methanol, at 60 degrees Celsius Stir for 2 hours, thin-layer chromatography (volume ratio: petroleum ether / ethyl acetate=1:1, main point Rf value 0.4) shows that the raw material has been consumed, the reaction solution is filtered, and the filter cake is washed with 100 ml of hot methanol , the filtrate was concentrated and then purified by silica gel column chromatography (petroleum ether ethyl acetate system, 10:1 to 2:1) to obtain compound 4 (3.00 g, 9.82 mmol, 65.86% yield) as a yellow solid.
Embodiment 3
[0075] Embodiment 3. Preparation of compound 5
[0076]
[0077] Compound 4 (0.10g, 0.33mmol) and 2-hydroxy-3-methoxybenzaldehyde (0.075g, 0.491mmol) were heated to reflux in 1.5ml of ethanol for 18 hours, and sodium borohydride (0.04 g, 0.98mmol)) and continued to stir for 6 hours, then quenched with 1 ml of methanol and 1 ml of water and continued to stir for 20 minutes, the mixture was filtered with celite, the filtrate was concentrated to dryness and purified by preparative HPLC Compound 5 was obtained.
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