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SrHPO4/BaHPO4催化合成2-甲基三乙烯二胺及其类似物

         

摘要

以2-甲基哌嗪及其类似物和2-氯乙醇为原料,采用气固相催化工艺,以SrHPO4/BaHPO4为催化剂,两步反应合成高收率、高纯度的2-甲基三乙烯二胺及其类似物,并考察了两步反应条件对目标产物产率的影响.较佳的合成条件为:第一步反应,n(2-甲基哌嗪及其类似物)∶n(2-氯乙醇)=1.0∶2.0,反应温度70℃,反应时间6h;第二步反应,预热器温度200℃,固定床反应温度340℃,进料量2 mL/min.2-甲基三乙烯二胺的两步反应产物收率84%,纯度98%以上;三乙烯二胺的两步反应收率88%,纯度98%以上.%2-Methyl-1,4-diazabicyclo [2.2.2] octane and its analogues with high yield and purity were synthesized from 2-methyl piperazine with its analogues and 2-chloroethanol in fixed bed with SrHPO4/BaHPO4 as the catalyst.The influence of two-step reaction conditions on the yield and content of products was studied.The reaction conditions of first step are that the optimal ratio between 2-methyl piperazine with its analogues and 2-chloroethanol was 1.0 ∶ 2.0 at 70 ℃ and reaction time was 6 h.The reaction conditions of second step are that the preheater temperature was 200 ℃ and optimal temperature of fixed bed was 340 ℃ with feed rate 2 mL/min.The total yield of 2-methyl-1,4-diazabicyclo[2.2.2] octane was 84% with the purity over 98% and the total yield of 1,4-diazabicyclo[2.2.2] octane was 88% with the purity over 98%.

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