化学合成。
化学合成
合成路线 1(1. 合成:62266-82-4)
产率:90%
合成条件:With bromine In dichloromethane at 20℃; for 3 h;
实验步骤:将溴(5.1mL,99.2mmol)滴加到3H-苯并噻唑-2-酮7(5g,33,1mmol)的DCM(200mL)溶液中,并将反应混合物在室温下搅拌3小时。 过滤沉淀物,用乙醚洗涤并干燥,得到8,为白色粉末(6.85g,90%);C7H4BrNOS;MW =230.1克/摩尔; 熔点229-231℃。 1 H NMR(300MHz,CDCl 3):δ7,03(d,1H,J = 8,9Hz); 7,43(dd,1H,J = 1.7Hz,8,9Hz); 7,85(d,1H,J = 1,7Hz)。 MS(ESI +)m / z 229.8 [M + H79Br] +,231.7 [M + H81Br] +。
参考文献:
- [1] Journal of Heterocyclic Chemistry, 1988, vol. 25, p. 1503 - 1509 [2] European Journal of Medicinal Chemistry, 2017, vol. 137, p. 310 - 326 [3] Monatshefte fur Chemie, 2011, vol. 142, # 1, p. 67 - 80 [4] European Journal of Medicinal Chemistry, 2015, vol. 92, p. 807 - 817 [5] Bollettino Scientifico della Facolta di Chimica Industriale di Bologna, 1944, vol. 5, p. 11,14, 16, 18 [6] Journal of the Chemical Society, 1930, p. 125,145 [7] European Journal of Medicinal Chemistry, 2015, vol. 92, p. 575 - 582