In the present study the potential of solketal transacetalization reaction has been demonstrated as an effective method of synthesis of acetals of glycerol and lipophilic carbonyl compounds (2‐ethylhexanal, n‐decanal, cyclopentanone, cyclohexanone). In solketal transacetalization with 2‐ethylhexanal reaction rate was significantly higher than of direct acetalization of glycerol both with and without a solvent because on the contrary to glycerol solketal is freely miscible with lipophilic compounds. Unlike the direct acetalization, reaction rate increased along with the temperature with no losses in equilibrium conversion. Furthermore, by stripping of by‐product acetone from the reaction zone we have succeeded in increasing the product yield in one‐pot synthesis to 97–98%, so that no further purification is needed. Finally, transacetalization was shown to be catalyzed with solid acids much more efficiently than the direct reaction (the cheap and eco‐friendly montmorillonite K‐10 catalyst was found to be the most active). Based on the regulations revealed, a green atom‐efficient synthetic protocol to obtain higher glycerol acetals and ketals has been proposed.

中文翻译：

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缩酮的反缩醛化：一条基于生物甘油的特种化学品的绿色路线

在本研究中，已经证明了缩酮缩醛化反应的潜力是一种合成甘油和亲脂性羰基化合物（2-乙基己醛，正癸醛，环戊酮，环己酮）的缩醛的有效方法。在有2-乙基己醛的酚缩醛缩醛化反应中，无论有无溶剂，甘油的直接缩醛化反应率都明显高于甘油的直接缩醛化，因为与甘油相反，solketal可以与亲脂性化合物自由混溶。与直接缩醛化不同，反应速率随温度的增加而增加，平衡转化率没有损失。此外，通过从反应区中汽提副产物丙酮，我们成功地将单釜合成中的产物收率提高到97-98％，因此无需进一步纯化。最后，结果表明，与直接反应相比，使用固体酸催化反式缩醛化要有效得多（发现廉价，环保的蒙脱石K-10催化剂活性最高）。根据揭示的法规，提出了一种绿色原子有效的合成方案，以获得更高的甘油缩醛和缩酮。