N,N-二烯丙基-N-羰丁氧甲基氯化铵的合成与表征

Synthesis and Characterization of N,N-Diallyl-N-carbobutoxy-methylammonium Chloride

以二烯丙基胺、氯乙酸丁酯和K2CO3为原料,合成了N,N-二烯丙基-N-羰丁氧甲基胺（DACBMA）,将油相与水相分离后用无水硫酸镁干燥,再减压蒸馏,收集157~161℃/1 333 Pa的馏分;然后将收集的馏分用6 mol/L的盐酸中和至油相消失,得到N,N-二烯丙基-N-羰丁氧甲基氯化铵（DACBMAC）溶液;或将其溶于无水乙醚,通入干燥氯化氢,可得到固体DACBMAC。结果表明,当n（二烯丙基胺）∶n（氯乙酸丁酯）∶n（K2CO3）=1.5∶1∶1,反应温度70℃,氯乙酸丁酯滴加时间60 m in,反应时间8 h时,DACBMA的收率为74.30%;将分离得到的水相和减压蒸馏得到的低沸点馏分回用,其收率可提高到83.23%;与干燥氯化氢季铵化相比,采用盐酸中和反应快,无尾气污染,但不能得到固体产物;DACBMAC收率达81.56%,比干燥氯化氢季铵化高10.51%。用元素分析、FTIR和1HNMR对中间产物和终产物的结构进行了表征。并已进行了1 L规模的扩试。

N, N-Diallyl-N-carbobutoxymethylamine （ DACBMA ） was synthesized using diallylamine, butyl chloroacetate and K2CO3 as raw materials. After separated from the water phase, the oil phase was dried by anhydrous magnesium sulfate and then collected 157 - 161 ℃/1 333 Pa cuts by the reduced pressure distillation to obtain DACBMA. The solution of N, N-diallyl-N- carbobutoxymethylammonium chloride （DACBMAC） was obtained by neutralizing the cuts using 6 mol/L hydrochloric acid till the oil phase disappeared. The DACBMAC solid was synthesized by ventilating anhydrous hydrogen chloride in DACBMA ethyl ether solution. The results show that,when n （diallylamine） ：n （ butyl chloroacetate） ：n （ K： CO3 ） = 1.5：1 ： 1, the adding time for butyl ehloroaeetate is 60 min, the reaction time is 8 h and the reaction temperature is 70 ℃, the yield of DACBMA is 74.30% and it increases to 83.23% by reusing the water phase and the lower boiling point cuts collected;Compared with quaternarization by anhydrous hydrogen chloride, the reaction neutralized by hydrochloric acid is quick with no pollution, but the solid product could not be obtained. The yield of DACBMAC is 81.56% which is 10. 51% higher than that of quaternarization by anhydrous hydrogen chloride. Structures of the in-process product and the product are characterized by elementary analysis, FTIR and ^1HNMR. The 1 L bench-scale research for this technology had been done.