香料羧酸糠醇酯合成的新方法

用糠醇、乙酸酐和丙酸酐为原料,Fe2(SO4)3.xH2O为催化剂,NaHCO3为缚酸剂,合成了乙酸糠醇酯和丙酸糠醇酯。考察了反应物料比、反应时间、催化剂和缚酸剂用量对收率的影响。合成乙酸糠醇酯的最佳条件为:物料配比n糠醇∶n乙酸酐∶nFe2(SO4)3.xH2O∶nNaHCO3=2∶2∶0.03∶2(摩尔比),室温下反应4 h;合成丙酸糠醇酯的最佳反应条件为:物料配比n糠醇∶n丙酸酐∶nFe2(SO4)3.xH2O∶nNaHCO3=2∶2∶0.04∶2(摩尔比),室温下反应4 h。乙酸糠醇酯和丙酸糠醇酯的收率分别为88.8%和90.2%。该反应条件温和、产率高,可用于工业化大规模生产。目标产物结构经IR、1H NMR表征得以证实。

Novel method for synthesis of perfume furfuryl carboxylate

Furfuryl carboxylate was synthesized from furfuryl alcohol,acetic anhydride and propionic anhydride by using hydrated ferric sulfate as catalyst and anhydrous sodium carbonate as acid-caputor.The effect of reaction time,reactant mole ratio,contents of catalyst and acid-caputor on product yield was investigated.The optimum reaction conditions for synthesis of furfuryl acetate were:mole ratio of furfuryl alcohol,acetic anhydride,hydrated ferric sulfate to anhydrous sodium carbonate is 2 ∶2 ∶0.03 ∶2,react for 4 h at room temperature.The optimum conditions for synthesis of furfuryl propionate were: mole ratio of furfuryl alcohol,propionic anhydride,hydrated ferric sulfate to anhydrous sodium carbonate is 2 ∶2 ∶0.04 ∶2,react for 4 h at room temperature.Under the above condition the yields of furfuryl acetate and furfuryl propionate were 88.8% and 90.2% respectively.The method had the advantanges of moderate reaction conditions,high yield and large scale production.The structures of the products were confirmed by IR and 1H NMR.