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α、ω-烷二醇的单保护衍生物是合成昆虫性信息素、前列腺素等天然产物的重要中间体。有关它的合成方法的研究,已引起了人们广泛的兴趣。1979年,James 等人首次报道了用连续抽提法进行对称二醇的选择性单酰化反应,并指出反应体系中水的用最是影响反应选择性的关键。然而,我们按文献[7]的配比多次重复,产率仅在50%左右,单酰化产物与双酰化产物之比小于10∶1。我们在文献[7]的基础上,采用经典的液-液提取法,用硫酸作催化剂,提高反应温度
Mono-protected derivatives of α, ω-alkanediols are important intermediates for the synthesis of natural products such as sex pheromones and prostaglandins. The research on its synthesis method has aroused widespread interest. In 1979, James et al. First reported the selective monoacylation of symmetrical diols by continuous extraction and pointed out that the most important factor influencing the selectivity of the reaction was the water used in the reaction system. However, we repeated many times according to the reference of [7], the yield was only about 50%, and the ratio of monoacylated product to bisacylated product was less than 10: 1. Based on the literature [7], we use the classical liquid-liquid extraction method and use sulfuric acid as catalyst to increase the reaction temperature