可聚合单体N,N-二甲基丙烯酰乙二胺的合成条件研究

Study on synthesis condition of polymerizable monomer N-[(dimethylamino) ethyl]acrylamide

利用丙烯酸和苯甲酰氯合成丙烯酰氯(AC),AC再与N,N-二甲基乙二胺(DMAEA)合成可聚合单体N,N-二甲基丙烯酰乙二胺。通过红外光谱和核磁共振谱证实产物的结构。考察原料的物质的量比、不同缚酸剂的用量与浓度、稀释N,N-二甲基乙二胺和丙烯酰氯的二氯甲烷的量、加料顺序对产品收率的影响,得出适宜的实验条件为:n(DMAEA)∶n(AC)=1∶1.2,缚酸剂w(NaOH)=25%的用量为25mL,稀释N,N-二甲基乙二胺和丙烯酰氯的二氯甲烷的量分别为80mL和45mL,加料顺序为先加N,N-二甲基乙二胺的二氯甲烷溶液,再加缚酸剂。在上述条件下,产品最高收率可达83%。

Acryloyl chloride（AC）was synthesized with acrylic acid and benzoyl chloride.N-[（dimethylamino） ethyl]acrylamide,a kind of polymerizable monomer,was prepared with（AC）and 2-dimethylaminoethylamine（DMAEA）.The product was identified by IR and 1H NMR.The effects of different reaction conditions（mass ratio of n（DMAEA） to n（AC）,kind and quantity of acid-binding agent,solvent usage and feeding sequence） on the yield of the product were investigated.Optimum reaction parameters for thus synthesis were obtained as follows.mass ratio of n（DMAEA） to n（AC） is 1∶1.2.25 mL NaOH solution（25%） is used as acid-caputor.The amount of dichloromethane for diluting DMAEA and AC is 80 mL and 45 mL,respectively.The feeding sequence is that acid-binding agent followed with dichloromethane.Under these reaction conditions,the yield of product is 83%.