4576-90-3, Isothiazole-3-carboxylic acid is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
To a stirred suspension of isothiazole-3-carboxylic acid (10.02 g, 77.6 mmol) in anhydrous te/f-butanol (80 ml_) and anhydrous toluene (120 ml_) was slowly added triethylamine (13.0 ml_, 93.12 mmol). The mixture was stirred at ambient temperature for 5 minutes and then diphenyl phosphoryl azide (18.42 ml_, 85.36 mmol) was added dropwise to it. The reaction mixture was stirred at ambient temperature for 1 h, gradually warmed to 85 C over 1 h, and then heated at 85 C with stirring for 7 h. After cooling to ambient temperature, the reaction mixture was diluted with ethyl acetate (150 ml_) and saturated aqueous sodium bicarbonate (150 ml_). The layers were separated and the aqueous layer was extracted with ethyl acetate (2 c 100 ml_). The combined organic layers were washed with water (150 ml_), brine (150 ml_), dried over magnesium sulfate, and filtered. Concentration of the filtrate in vacuo provided a residue, which was purified by column chromatography, eluting with a gradient of 0 to 10% of ethyl acetate in heptane. Further purification by column chromatography, eluting with a gradient of 0 to 10% of ethyl acetate in dichloromethane, afforded the title compound as a colorless solid (10.33 g, 66% yield): 1H NMR (400 MHz, CDCI3) d 8.56 (dd, J = 4.9, 0.6 Hz, 1 H), 8.11 (s, 1 H), 7.66 (d, J = 4.9 Hz, 1 H), 1.53 (s, 9H); MS (ES+) m/z 201.1 (M + 1).
The synthetic route of 4576-90-3 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; XENON PHARMACEUTICALS INC.; FOCKEN, Thilo; BURFORD, Kristen Nicole; LOFSTRAND, Verner Alexander; WILSON, Michael Scott; ZENOVA, Alla Yurevna; (121 pag.)WO2019/241533; (2019); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com