化学合成。是有机中间体,可用于合成基于空间光诱导电子转移(SPET)的新型探针。
化学合成; 有机中间体
合成路线 1(1. 合成:22952-24-5)
产率:72%
合成条件:With chromium(VI) oxide; sulfuric acid In water at 20℃; for 24 h;
实验步骤:向溶液中将三氧化铬(20.4g,0.204mol)的水(150mL)溶液在冰浴中逐滴加入浓硫酸(190mL)。 加入2-甲基-5-硝基苯磺酰胺(10g,46.3mmol),将混合物在室温下搅拌24小时。 过滤混合物,残余物用水洗涤,溶解在碳酸氢钠溶液中并在真空下过滤。 将滤液用浓HCl酸化。 过滤沉淀的产物并用大量冷水洗涤后,将其在40℃的真空烘箱中干燥。 得到白色粉末,产率72%。 熔点205.6-205.8℃,(lit.36 205-207℃); IR:3103,1720,1608,1541,1354,1340,1184,1128cm -1; 1H NMR(DMSO-d6,300MHz)δ/ ppm:8.02(1H,d,J = 8.5Hz),8.56(1H,d,J = 8.2Hz),8.71(1H,s),10.2(1H,br ,NH); 13C NMR(DMSO-d6,75MHz)δ/ ppm:117.2,126.4,129.8,135.2,143.0,151.7,162.2。
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