N，N，N′，N′-四烯丙基乙二胺的合成与表征

SYNTHESIS AND CHARACTERIZATION OF N,N,N',N'TETRAALLYLETHYLENEDIAMINE

实验以乙二胺、烯丙基氯和碱为原料,分二步合成了N,N,N′,N′-四烯丙基乙二胺(TAEDA)。考察了乙二胺、烯丙基氯和碱的摩尔比、反应温度、反应时间和相转移催化剂用量等因素对TAEDA收率的影响。合成TAEDA较佳工艺条件为:第一步,n(乙二胺):n(烯丙基氯):n(碱)=1:2.2:2.1,反应温度60℃,反应时间6 h。第二步,烯丙基氯和碱的用量与第一步相同,反应温度70℃,反应时间9 h,相转移催化剂的加入量为烯丙基氯质量的1.8%;反应后将所得水相和低沸点馏分返回参加下一轮反应,TAEDA收率由69.75%提高至79.29%。

N,N,N′,N′-tetraallylethylenediamine （TAEDA） was synthesized by a two-step method using ethylenediamine, allyl chloride and alkali as raw materials. The effects of the molar ratio of ethylenediamine, allyl chloride and alkali, the reaction temperature, the reaction time and the dosage of phase transfer catalyst on the yield of TAEDA were investigated. The synthetic conditions were optimized by orthogonally arranged experiments and the structure of TAEDA was characterized by FTIR, 1HNMR and elementary analysis. The optimal conditions were found as follows： for the first step, n （ethylenediamine） ： n（allyl chloride） ： n（alkali） = 1 ： 2.2 ： 2.1, reaction temperature 60℃ and reaction time 6h; For the second step, the dosages of allyl chloride and alkali were the same as the first step, the reaction temperature was 70 ℃, the reaction time was 9 h and the dosage of the phase transfer catalyst was 1.8% of the mass of allyl chloride. The yield of TAEDA increased from 69.75% to 79. 29% by reusing the water phase and the lower boiling point cuts collected.