甲氧基香茅醛合成工艺研究

以香茅醛为原料,经二甲胺羰基保护、硫酸催化条件下甲氧基化、氢氧化钠中和合成甲氧基香茅醛。考察了反应温度、反应时间、投料比等工艺条件对产品收率的影响。实验研究得到了最优的合成工艺条件为:胺化反应二甲胺与香茅醛摩尔比为2∶1,反应温度10~15℃,反应时间3 h。甲氧基化反应硫酸浓度为100%,甲醇∶硫酸∶烯胺的摩尔比为15∶5∶1,反应温度15~18℃,反应时间2 h。产品总收率47.6%。反应工艺简单,条件温和,原料易得,便于工业化。产品经IR1、H NMR、GC/MS、元素分析确证结构。

Study on Synthesis of Methoxycitronellal

Methoxycitronellal was synthesized by the carbonyl protection of dimethylamine,alkoxylation of citronellal with sulfuric acid as catalyst and final neutralization with sodium hydroxide.The effect of reaction temperature,reaction time and the ratio of raw materials on the yield of product was studied.The results showed the optimum conditions of the amination reaction are: the molar ratio of dimethylamine∶citronellal is 2∶1,reaction temperature is 10～15 ℃ and reaction time is 3 h.Furthermore,the optimum conditions of methoxycitronellal reaction are: the concentration of sulfuric acid is 100%,the molar ratio of methyl alcohol∶sulfuric acid∶enamine is 15∶5∶1,reaction temperature is 15～18 ℃ and reaction time is 2 h.The final yield of product is 47.6%.The reaction is simple, the raw materials are easily available and the production in industry is easy to operate.The structure of the product was characterized by IR,()~1H NMR, GC/MS and elemental analysis.