摘要
以Delépine伯胺制备方法为依据,用无水乙醇代替氯仿做溶剂,通过烯丙基氯与乌洛托品反应制备烯丙基胺.详细考察了酸碱用量、催化剂用量、物料配比及溶剂用量对反应的影响,发现在n(C3H7Cl)∶n(C6H12N4)=0.95∶1,x(KI)=2.5%,40℃,t=10h,n(NaOH)∶n(HCl)∶n(C6H12N4)=4∶4∶1的条件下,产品烯丙基胺收率为86.6%,烯丙基氯转化率达100%.产品经GC-MS及IR分析,结构正确.
The synthesis of allylamine based on the method of Delépine amine by the reaction of allylchloride in ethanol and hexamethylenetetramine in the presence of KI was investigated. The effects of various factors on the reaction, such as the HCl and NaOH dosage, catalyst dosage, molar ratio of raw materials, ethanol dosage were determined. The allylamine was identified by GC-MS and IR. The conversion of allylchloride is 100% and the yield of allylamine is 86.6%, while the reaction temperature is 40 ℃,the molar ratio of allylchloride to hexamethylenetetramine is 0.95∶1, the catalyst dosage based on hexamethylenetetramine is 2.5%, the reaction time is 10 h and the molar ratio of NaOH and HCl to hexamethylenetetramine is 4∶4∶1.
出处
《大连理工大学学报》
EI
CAS
CSCD
北大核心
2004年第2期224-227,共4页
Journal of Dalian University of Technology
基金
国家自然科学基金资助项目(20076006).
