2-(Substituted phenyl)-4,4,5,5-tetramethyl-1-hydroxy-imidazoline, its synthesis, activity and application
A technology of tetramethylimidazoline and hydroxyl group, which is applied in the application field of preparing antithrombotic drugs, thrombolytic drugs and drugs for treating ischemic stroke
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Embodiment 1
[0022] Embodiment 1 prepares 2,3-dimethyl-2,3-dinitrobutane
[0023] Add 130mL of 6N NaOH solution to 69.0g (0.78mol, 70mL) of 2-nitropropane successively under ice bath and stirring, 20mL (0.38mol, slowly dropwise, within 1 hour) of Br 2 and 240 mL of ethanol. The reaction compound was refluxed at 90°C for 3 hours, during which a flaky precipitate appeared. The reaction solution was poured into 800mL of ice water while it was hot, and 49.0g (73%) of the title compound was obtained by filtration as colorless flaky crystals. ESI-MS(m / e):177[M+H] + .
Embodiment 2
[0024] Embodiment 2 prepares 2,3-dimethyl-2,3-dihydroxyaminobutane
[0025] 7.00g (40mmol) 2,3-dimethyl-2,3-dinitrobutane and 4.00g NH 4 Dissolve Cl in 80 mL of 50% aqueous ethanol, stir under ice bath, and add 16.00 g of zinc powder in batches within 3 hours. After the zinc powder was added, the reaction mixture was stirred at room temperature for 3 h, filtered with suction, and the filter cake was repeatedly washed with 50% aqueous ethanol. Combine the filtrate and washing liquid, adjust the pH to 2 with concentrated hydrochloric acid, and concentrate under reduced pressure to obtain a slurry. Dissolve the slurry with a small amount of 50% ethanol aqueous solution, add an appropriate amount of potassium carbonate, mix well, put it into a Soxhlet extractor, use dichloromethane as the extractant, extract at 60°C for 6 hours, concentrate the extract under reduced pressure, and use the residue Trituration with petroleum ether gave 2.07 g (35%) of the title compound as a colorl...
Embodiment 3
[0026] Example 3 Preparation of 2-(3-carboxy-4-hydroxyphenyl)-1,3-dihydroxy-4,4,5,5-tetramethylimidazole
[0027] Dissolve 1.48g (10mmol) of 2,3-dimethyl-2,3-dihydroxyaminobutane in a small amount of methanol at room temperature, add 2.0g (12mmol) of 3-carboxy-4-hydroxybenzaldehyde, and react for 12 hours. Filtration afforded 2.07 g (70%) of the title compound as a colorless powder. ESI-MS(m / e):298[M+H] + .
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