茴香脑臭氧化制备茴香醛

以茴香脑为原料,乙酸和环己烷的混合物做溶剂,臭氧化法制备茴香醛。考察了溶剂、臭氧化时间、还原剂用量、还原分解时间和还原温度对反应结果的影响,初步探讨了臭氧化反应级数。优化的工艺条件为,m(乙酸)∶m(环己烷)=1∶4,臭氧化时间为100min,n(NaHSO3)/n(茴香脑)=1.1,还原分解时间60 min,还原温度80℃。在此条件下,产品收率≥84%,纯度≥98%。

Preparation of Anisaldehyde from Anethole by Ozonolysis Reaction

The preparation of anisaldehyde by ozonolysis reaction from anethole was studied.Using the mixture of acetic acid and cyclohexane as solvent,the effects of factors such as amount of solvent,ozonolysis temperature, ozonolysis time,amount of reductant and reduction decomposition time on reaction results were examined.The reaction order was also studied.The obtained optimum conditions were m(acetic acid): m(cyclohexane)= 1∶4,ozonolysis time 100 min,n(NaHSO3)/n(anethole) = 1.1,reduction decomposition time 60 min,reduction temperature 80 ℃.Under above conditions,the yield of product was over 84% with the purity≥98%.