化学合成
化学合成
路线1:以二甲基亚磷酸酯、三乙胺和多聚甲醛为原料合成
- 步骤:将搅拌的二甲基亚磷酸酯(10.0ml,109mmol)、三乙胺(1.5ml,10.9mmol)和多聚甲醛(3.26g)的混合物在100℃油浴(外部温度)中加热;2.5小时后冷却至室温,真空浓缩,通过快速柱色谱法(洗脱液:乙酸乙酯/甲醇95:5)纯化残余物,得到无色油状物标题化合物(9.41g)。
- 条件:反应温度100℃;反应时间2.50h。
- 收率:62%。
- 表征数据:1H NMR(400MHz,CDCl3)δppm 4.32(1H,br s),3.95(2H,d,J=6Hz),3.83(3H,s)和3.81(3H,s);31P{1H} NMR(400.1MHz,CDCl3)δppm 27.8;13C NMR(100.6MHz,CDCl3)δppm 53.5、56.0和57.6。
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