第 52 卷第 4 期Vol. 52 No. 4
2022 年 8 月Aug 2022

所属栏目:功能材料

N-(4-乙氧基羰基苯基)-N-甲基-N-苯基甲脒的合成
刘 柳,孟纪文 (中昊(大连)化工研究设计院有限公司,辽宁 大连 116023)
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Al2O3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Al2O3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。
关键词:紫外线吸收剂;4-氨基苯甲酸乙酯;原甲酸三甲酯;N-甲基苯胺;合成
中图分类号:TQ246  文献标识码:A  文章编号:1009-9212(2022)04-0076-03
Synthesis of N-(4-Ethoxycarbonylphenyl)-N′-methyl-N′-phenyl Formamidine
LIU Liu, MENG Ji-wen (China Haohua (Dalian) Research & Design Institute of Chemical Industry Co., Ltd., Dalian 116023, China)
Abstract:N-(4-Ethoxycarbonylphenyl)-N'-methyl-N'-phenyl formamidine was synthesized through one step from ethyl 4-aminobenzoate, trimethyl orthoformate and N-methylaniline with active Al2O3 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 Al2O3 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.
Key words:ultraviolet absorber; ethyl 4-aminobenzoate; trimethyl orthoformate; N-methylaniline; synthesis
作者简介:刘 柳(1982—),女,辽宁锦州人,工程师,硕士,研究方向:药物中间体及精细化学品(E-mail:postboymjw@163.com)。
收稿日期:2022-05-05