2-Amino-7-substituted benzothiazole compounds, preparation method and use thereof
A technology of benzothiazole and compounds, applied in the field of medicinal chemistry, can solve the problems of high cost, high medical expenses, and unsatisfactory effects, and achieve the effects of simple post-processing, high yield, and short reaction steps
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[0056] The synthesis of embodiment 12-amino-7 trifluoromethylmercaptobenzothiazole
[0057] Dissolve 0.01mmol of 3-trifluoromethylmercaptoaniline in 10mL of acetic acid, add 30mmol of potassium thiocyanate and stir for 25 minutes. 13 mmol of bromine was dissolved in 0.7 mL of acetic acid, slowly added to the above-mentioned reactant, the reaction temperature in a water bath was 20°C, stirred overnight, filtered, and the precipitate was washed 3 times with 25 mL of ethyl acetate. Combine the filtrate and washing liquid, alkalinize it with ammonia solution, wash twice with 120mL concentrated brine, concentrate to 20mL, apply flash chromatography, and elute with n-hexane: acetone 5:1-4:1 (v / v). The eluate was collected and the solvent was evaporated to obtain 1.38 g of 2-amino-7-trifluoromethylmercaptobenzothiazole with a yield of 55%. 1 H-NMR (CDCl 3 , 500MHz), 4.14(brs, 2H), 6.79(dd, J=8.5Hz, J=2.5Hz, 1H), 7.06(d, J=2.5Hz, 1H), 7.54(d, J=8.0Hz, 1H ); ESI-MS (m / z, %): 249.26 ...
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