化学合成。
医药
合成路线 1(1. 合成:6972-27-6)
产率:92.3%
合成条件:for 6 h; Reflux; Large scale
实验步骤:将1,3-二甲基巴比土酸(化合物SM1)(7kg,44.9mmol)溶于120kg磷酰氯(POCl 3)中。 向它缓慢滴水(2.2千克,22立方米)。 下降后。 缓慢加热至回流6小时; 高效液相色谱监测,反应结束后,将反应液慢慢倒入大量冰水(100L)中,再用50L二氯甲烷萃取2次,合并有机相,饱和盐水洗涤(20L),无水硫酸钠干燥 ,过滤,浓缩有机相,真空干燥得到黄色固体7.2kg,SM2为化合物,收率92.3%。
参考文献:
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