用于医药和农药领域,具体用途未详细说明。
医药; 农药
合成路线 1(1. 合成:1446507-38-5)
产率:71%
合成条件:Stage #1: at 30 - 35℃; Large scale Stage #2: With titanium(IV) tetraethanolate In ethanol at 30 - 35℃; Large scale Stage #3: With sodium ethanolate In ethanol at 55 - 65℃; for 3 h; Large scale
实验步骤:100801将6-(三氟甲基)吡啶甲酸甲酯(50g,244mmol,1.0当量)和缩二脲(30.2g,293mmol,1.20当量)在750mL EtOH中的混合物在30-35℃下搅拌10-20mm。 加入四乙氧基钛(Ti(OEt)4,27.8g,122mmol,0.5当量)并在30-35℃下搅拌30-60ml EtONa的EtOH溶液(350g,19%wt,978mmol,4.0eq) 加入),将反应混合物在55-65℃加热3小时。 浓缩反应混合物,冷却至室温,并用700mL水稀释。 加入浓HCl溶液以将pH值调节至pH1。 加入二氯甲烷(DCM,700mL),将浆液在20-30℃下搅拌5-7小时。 过滤收集固体,将滤饼依次用6N HCl洗涤两次,用水洗涤两次,用DCM洗涤一次。 将湿滤饼在50-60℃下真空干燥,得到6-(6-(三氟甲基)吡啶-2-基)-1,3,5-三嗪-2,4(1H,3H) - 二酮作为关闭 白色固体(45.0g,174mmol,71%收率)。
参考文献:
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