化学合成。
化学合成
合成路线 1(1. 合成:15456-86-7)
产率:87%
合成条件:With hydrazinium sulfate In water at 100℃; for 19 h;
实验步骤:在搅拌下将硫酸肼(2.25g,17,2mmol)溶解在沸水(20mL)中。 通过加料漏斗向该溶液中逐滴加入溴代马来酸酐(2.6mL,28.2mmol),将混合物在回流下加热(100℃)19小时,然后冷却至环境温度。 在中等玻璃料烧结玻璃漏斗上过滤所得白色沉淀,用丙酮(3×5ml)洗涤,真空空气干燥,得到所需产物4-溴-1,2-二氢哒嗪-3,6-二酮( 2.85g),白色粉末,87%收率(重量分析),熔点262℃。
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