化学合成。
化学合成
合成路线 1(1. 合成:1034667-22-5)
产率:88%
合成条件:With hydrazine In butan-1-ol for 4 h; Heating / reflux
实验步骤:向化合物4a(50g,321.7mmol)的1-丁醇(1L)溶液中加入一水合肼(150mL,3.2mol),并将混合物回流4小时。 将混合物冷却至室温并浓缩。 将沉淀物依次用水(2x)和Et 2 O(2x)洗涤,真空干燥过夜,得到化合物5a(44g,88%),为黄色固体。 1H NMR(DMSO-d6,300MHz):δ5.53(s,2H); 7.94(dd,IH); 8.35(dd,IH); 12.02(s,IH)。
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