二烯丙基乙胺的合成

Synthesis of Diallylethylamine

以乙胺、烯丙基氯和碱为原料合成了二烯丙基乙胺,其结构经1H NMR,FT-IR和元素分析表征。考察了反应物摩尔比、反应温度、反应时间和相转移催化剂用量对收率的影响,采用正交实验设计法对工艺条件进行了优化。较佳的反应条件为:乙胺370 mmol,n(乙胺)∶n(烯丙基氯)∶n(NaOH)=1.0∶2.1∶2.1,PEG-6005 mol%,第一段于42℃反应6 h;第二段于60℃反应7 h,收率71.58%。回用分液所得水相和减压蒸馏所得低沸点馏分,能回收存在于水相和低沸点馏分中的中间产物和产物,收率由71.58%提高到83.66%。

Diallylethylamine was synthesized from ethylamine, allyl chloride and alkali. The structure was characterized by ＇ H NMR, IR and elemental analysis. The effects of the molar ratio of reactants, the reaction temperature and time, and the dosage of phase transfer catalyst on the yield were investigated. The reaction conditions were optimized by orthogonal design method. The optimum conditions were as follows： ethylamine was 370 mmol ; n （ ethylamine ） ： n （ allyl chloride） ： n （ NaOH ） was 1.0 ： 2.1 ： 2.1 ; PEG-600 was 5 mol% ; the first stage reaction was carried out at 42 ℃ for 6 h and the rsecond stage reaction was at 60℃ for 7 h. The aqueous phase and light distillate were reused and the yield increased from 71.58% to 83.66%.