化学合成。
化学合成
合成路线 1(1. 合成:188057-26-3)
产率:95%
合成条件:With iodine; sodium carbonate In water at 20℃; for 48 h;
实验步骤:向上述物质(15.48g,119mmol)和Na 2 CO 3(26.56g,251mmol)的水(300mL)溶液中加入碘(30.3g,119mmol)。 将反应混合物在室温下搅拌直至碘颜色消失,约。 48小时 用1N HCl水溶液将溶液调节至pH = 5,并用乙酸乙酯萃取。 用饱和NaCl水溶液洗涤有机层,用Na 2 SO 4干燥,并真空浓缩。 所得白色固体用甲醇重结晶,得到17.8g(95%)标题化合物。 MS(m / e):256(M +); 计算值C5H3ClINO:理论值:C,23.51; H,1.18; N,5.48; 实测值:C,23.72; H,1.19; N,5.45。
参考文献:
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