化学合成。
化学合成
合成路线 1(1. 合成:74173-77-6)
产率:95%
合成条件:With tri-n-propylamine; trichlorophosphate In toluene at 20 - 110℃;
实验步骤:步骤B:2,4-二氯-6-硝基 - 喹唑啉的制备。 将磷酰氯(6.64mL,72.6mmol)加入到6-硝基-1H-喹唑啉-2,4-二酮(5.01g,24.2mmol)的甲苯(100mL)悬浮液中,并将反应混合物加热至55℃。 在25分钟内从加料漏斗滴加三正丙胺(12.1mL,63.9mmol)。 将反应混合物加热至110℃,保持6小时,在室温下搅拌4天,然后移液至水(75mL)中并剧烈搅拌1小时。 将两层过滤并分离。 将有机层用盐水(30mL)洗涤,干燥(MgSO 4)并浓缩,在高真空下24小时后得到标题化合物(3.79g,67%收率,95%纯度)。 该化合物不产生MS数据。 1 H NMR(600MHz,CDCl 3):9.18(d,J = 2.4Hz,1H),8.75(dd,J = 9.2,2.5Hz,1H),8.18(d,J = 9.2Hz,1H)。
参考文献:
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