摘要
2-氨基乙基呋喃是一种重要的医药中间体。以糠醛和硝基甲烷为起始原料,经过缩合、双键加成及还原反应制备了2-氨基乙基呋喃,GC纯度大于99%,总收率为62.2%,其化学结构经MS、^(1)H NMR和^(13)C NMR确证。探讨了缩合反应中硝基甲烷的用量对化合物3收率的影响,当n(硝基甲烷)∶n(糠醛)=1∶1时,产物收率最高,达到82.6%。考察了硼氢化钠的用量对化合物4收率的影响,当n(硼氢化钠)∶n(化合物3)=2∶1时,产物收率最高,达到88.6%。考察了甲酸铵的用量对目标产物收率的影响,当n(甲酸铵)∶n(化合物4)=4∶1时,还原反应收率最佳,达到85.0%。实验结果表明此方法操作简单、反应条件温和、适用于工业化生产。
2-Furan-2-yl-ethylamine is an important pharmaceutical intermediate.It was synthesized from 2-Furaldehyde and nitromethane by condensation,addition and reduction reaction.The GC purity was more than 99%,and the total yield was 62.2%.The structure was confirmed by MS,^(1)H NMR,^(13)C NMR.The effect of the amount of nitromethane on the yield of intermediate compound 3 was discussed,when n(nitromethane)∶n(2-Furaldehyde)=1∶1,the yield of compound 3 by condensation reaction was up to 82.6%.The effect of the amount of NaBH 4 on the yield of intermediate compound 4 was discussed,when n(sodium borohydride)∶n(compound 3)=2∶1,the yield of compound 4 by addition reaction was up to 88.6%.The amount of ammonium formate in reduction reaction were discussed,when n(ammonium formate)∶n(compound 4)=4∶1,the yield of target compound 1 could reach 85.0%.The experimental results showed that the method was simple,mild and suitable for industrial production.
作者
吕列超
万霞
张文超
邵翀
Lyu Liechao;Wan Xia;Zhang Wenchao;Shao Chong(Changzhou Jiade Pharmaceutical Technology Co.,Ltd.,Changzhou 213159,China;Jiangsu Agrochem Laboratory Co.,Ltd.,Changzhou 213022,China)
出处
《山东化工》
CAS
2023年第11期26-28,共3页
Shandong Chemical Industry
关键词
2-氨基乙基呋喃
中间体
糠醛
硝基甲烷
合成
2-furan-2-yl-ethylamine
intermediate
2-furaldehyde
nitromethane
synthesis