Guerbet十四醇的合成与表征

Synthesis and Characterization of Guerbet Tetradecyl Alcohol

以正庚醇为原料 ,通过Guerbet反应合成Guerbet十四醇 (2 戊基壬醇 ,C14 GA)。用IR、NMR和元素分析测定了C14 GA的结构 ,并研究了反应温度和用料比对其产率的影响。实验结果如下 :(1)在较优化的反应条件下 (正庚醇的总加入量为 1mol,在实验过程中 ,先加入 1/ 3mol庚醇和 1/ 4mol的KOH ,在 16 0℃下反应 2h ,然后再加入剩下的 2 / 3mol庚醇和 4g 5 %Pd -C催化剂 ,在 15 5℃下反应 6h)合成产物 ,其产率可达到 5 4 2 0 % ;(2 )所合成的产物与试图要得到的Guerbet十四醇 (2 戊基壬醇 ,C14 GA)含有相同的基团 (2×—CH3、10×—CH2 —、1×CH、1×—CH2 —O—和 1×—OH) ,而且 ,所合成的产物中 ,w (C) =79 0 6 % ,w (H ) =13 6 2 % ,与从Guerbet十四醇分子式计算的理论值w(C) =78 5 0 % ,w (H) =14 0 1%基本一致。可见所合成的产物正是Guerbet十四醇 (C14 GA)

Guerbet alcohol(2 pentylnonyl alcohol,C 14 GA) was synthesized from n heptanol by Guerbet reaction.The structure of C 14 GA was identified by IR,NMR and elementary analysis.The effects of reaction temperature and ratio of reactants on the yield of C 14 GA were studied.The experimental results are as follows.(1)The yield of the synthesized product can reach 54 20% under suitable reaction conditions.A first,1/3 mol n heptanol and 1/4 mol KOH reacted at 160 ℃ for 2 h.Then,2/3 mol n heptanol and 4 g 5% Pd-C catalyst were added and the reaction proceeded at 155 ℃ for 6 h.(2)The synthesized product contained the same groups (2×CH 3,10×CH 2,1×CH,1×CH 2-O- and 1×OH) as Guerbet tetradecyl alcohol does.Moreover,in the synthesized product, w (C) =79 06% and w (H)=13 62%,which agree with the corresponding calculated values of Guerbet tetradecyl alcohol formula.Therefore the synthesized product is proved to be Guerbet tetradecyl alcohol (C 14 GA).