合成E-10-羟基-2-癸烯酸的新方法

以1，8-辛二醇（1）为起始原料，经4步反应合成了（E）-10-羟基-2-癸烯酸，其结构经¹H NMR, ¹³C NMR和MS确证。考察了乙酰氯、缚酸剂种类及其用量［r=n（1）: n（乙酰氯）: n（缚酸剂）］对8-乙酰氧基-1-辛醇（2）收率的影响以及反应温度、三乙胺滴加温度、低温停留时间对8-乙酰氧基辛醛（3）收率的影响。结果表明：以三乙胺为缚酸剂，r=1.0 : 1.1 : 2.0时，2产率达78%；反应温度为-65 ℃、三乙胺滴加温度低于-50 ℃、低温反应3 h， 3产率达97%。

Novel Synthesis of E-10-Hydroxy-2-decanoic Acid

(E)-10-hydroxy-2-decenoic acid was synthesized by a four-step reaction using 1,8-octanediol(1) as starting material.The structure was confirmed by 1H NMR,13C NMR and MS.Effects of acetyl chloride, acid acceptors and its amount r=n(1) ∶n(acetyl chloride)∶n(acid acceptors)] on 8-acetoxy-1-octanol(2), reaction temperature, adding triethylamine temperature and retention time at low temperature on 8-acetyl aldehyde(3) were investigated.The results showed that using triethylamine as acid acceptor and r=1.0 ∶1.1 ∶2.0, the yield of 2 was 78%.Reacting at-65 ℃, dropping triethylamine below-50 ℃, and reaction at-50 ℃ for 3 h, the yield of 3 was up to 97%.