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作 者:刘柳 孟纪文 LIU Liu;MENG Ji-wen(China Haohua(Dalian)Research&Design Institute of Chemical Industry Co.,Ltd.,Dalian 116023,China)
机构地区:[1]中昊(大连)化工研究设计院有限公司,辽宁大连116023
出 处:《精细化工中间体》2022年第4期76-78,83,共4页Fine Chemical Intermediates
摘 要:以4-氨基苯甲酸乙酯、原甲酸三甲酯、N-甲基苯胺为原料,活性Al_(2)O_(3)为催化剂,一步合成了N-(4-乙氧基羰基苯基)-N'-甲基-N'-苯基甲脒。考察了原料配比、催化剂种类、温度和时间对反应的影响。优化的工艺条件为:n(对氨基苯甲酸乙酯)∶n(原甲酸三甲酯)∶n(N-甲基苯胺)=1.00∶1.10∶1.05,活性Al_(2)O_(3)用量为5 g,反应温度为60℃,反应时间为4 h,产品收率为90.5%,催化剂循环使用4次反应活性未见明显下降,具有较好的稳定性。N-(4-Ethoxycarbonylphenyl)-N'-methyl-N'-phenyl formamidine was synthesized through one step from ethyl 4-aminobenzoate,trimethyl orthoformate and N-methylaniline with active Al_(2)O_(3)as catalyst.The effects of raw material ratio,catalyst type,temperature and time on the reaction were investigated.The optimized process conditions were as followings:n(ethyl 4-aminobenzoate)∶n(trimethyl orthoformate)∶n(N-methylaniline)was 1.00∶1.10∶1.05;the active Al_(2)O_(3)dosage was 5 g;the reaction temperature was 60℃;the reaction time was 4 h.Under the above conditions,a yield of 90.5%was obtained.The catalyst was recycled for 4 times with good stability.
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