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二茂铁经酰化反应合成的乙酰基二茂铁(或双乙酰基二茂铁),含有少量未反应的二茂铁和酰化产物自身缩合生成的黑色胶状物。用有机溶剂(环己烷等)提纯多次,这些胶状物也很难除尽,且操作繁琐,得率和纯度都较低。本方法是将粗反应产物先用热水溶解进行重结晶,过滤和干燥后,用环己烷重结晶一次,所得产物的得率和纯度都比较高。提纯后的乙酰基二茂铁m.p.85.6～86.1℃,元素分析值与理论计算值相符合,红外光谱与文献报道的一致,得率为71.2％。双乙酰基二茂铁的提纯结果也很好。作者认为,反应产物在用热水溶解提纯过程中,黑色胶状物发生水解,又生成原酰化产物。
Acetylferrocene (or diacetylferrocene) synthesized by acylation of ferrocene contains a small amount of unreacted ferrocene and a dark gum formed by condensation of the acylated product itself. Purified multiple times with organic solvents (cyclohexane, etc.), these jelly also difficult to remove, and cumbersome to operate, yield and purity are lower. In the method, the crude reaction product is first dissolved in hot water to be recrystallized, and after filtration and drying, recrystallization from cyclohexane is performed once to obtain a product with relatively high yield and purity. The purified acetyl ferrocene m.p. 85.6 ~ 86.1 ℃, elemental analysis and theoretical calculations are consistent with the infrared spectra reported in the literature, the yield was 71.2%. The purification of diacetyl ferrocene is also very good. The authors believe that the reaction product in the hot water purification process, the black jelly hydrolyzed, but also generate the original acylation product.