环己烯臭氧化合成1,6-己二醛

1,6-adipaldehyde synthesized by cyclohexene ozonolysis

以环己烯为原料,采用Zn-CH_3COOH为还原剂,经臭氧氧化和还原分解得到1,6-己二醛。讨论溶剂种类、溶剂用量、反应温度、氧气流量、氧化反应时间、还原剂种类、还原分解时间、还原剂用量对环己烯臭氧化合成1,6-己二醛反应的影响。得到较佳反应条件(以0.05 mol环己烯计)为:采用冰乙酸和1,2-二氯乙烷混合溶剂,冰乙酸6 g,1,2-二氯乙烷30 mL,臭氧化温度(0～5)℃,O_2流量(100～200) mL·min^(-1),臭氧化反应时间180 min,活化锌粉为还原剂,n(锌粉)∶n(环己烯)=1∶1,还原分解时间60 min。在该反应条件下,重复实验三次,1,6-己二醛平均收率可达61.6%。

1,6-adipoaldehyde was synthesized by ozone oxidation and reduction decomposition using cyclohexene as material,Zn-CH 3 COOH as reducing agent.The effects of solvent,amount of solvent, reaction temperature,flowrate of oxygen,ozonization time,reducing agent,restore decomposition time,and amount of reducing agent were investigated.The appropriate reaction conditions (based on 0.05 mol cyclohexene ) were that mixture of aceticacid and sym-dichloroethane was solvent,amount of aceticacid was 6 g,amount of sym-dichloroethane was 30 mL,reaction temperature was (0-5)℃,flowrate of oxygen was (100-200) mL·min ^-1 ,ozonization time was 180 min,activated zinc powder was reducing agent , n (zinc powder): n (cyclohexene)=1 ∶1,restore decomposition time was 60 min.Under the above conditions,1,6-adipaldehyde average yield of three times of eartion was about 61.6%.