山苍子油直接合成柠檬腈

Direct Synthesis of Lemonile from Litsea Cubeba Oil

用山苍子油直接同硫酸羟胺反应生成柠檬肟,再加入乙酐和相转移催化剂脱水得到柠檬腈.通过正交实验确定了柠檬肟合成的最佳工艺条件为:n(山苍子油)∶ n(羟胺)=1∶ 1.5,pH=5.5～6.0,反应温度45～50 ℃,反应时间3.5 h,柠檬肟的产率为90.1%.柠檬腈合成工艺为:n(柠檬肟)∶ n(乙酸酐)＝1∶ 4,反应温度125～130 ℃,反应时间1.0 h,柠檬腈的产率为78.0%.最后用IR、UV、GC谱对产品做了分析.

Litsea cubeba oil reacted with hydroxylamine sulfate to give citral oxime,which by dehydration with acetic anhydride in the presence of phase transfer catalyst gave lemonile.The optimum technological conditions for synthesis of citral oxime were:n(Litsea cubeba oil)∶n(hydroxylamine sulfate)=1∶1.5,pH=5.5～6.0,reaction temperature 45～50 ℃ and reaction time 3.5 h.Yield of citral oxime was 90.1%.The optimum technological conditions for synthesis of lemonile were:n(citral oxime)∶n(acetic anhydride)=1∶4,reaction temperature 125～130 ℃ and reaction time 1.0 h.Yield of lemonile was 78.0%.The product was investigated by FTIR,UV and GC.