武汉工程大学学报2018，Vol.40Issue(1)：17-22,6.DOI:10.3969/j.issn.1674-2869.2018.01.001
一种草铵膦新型中间体的合成和表征
Synthesis and Characterization of 2-acetamido-4-[hydroxy(methyl) phosphonyl]but-2-enoic acid,A New Intermediate of Glufosinate-Ammonium
摘要
Abstract
The 2-acetamido-4-[hydroxy(methyl)phosphonyl]but-2-enoic acid,an intermediate for producing glufosinate-ammonium,was synthesized with diethyl acetamidomalonate as a start material through hydrolysis and condensation reactions. The yield of monoethyl ester was 85.3％ by hydrolysis with 1.02:1 mole ratio of sodium hydroxide to diethylacetamidomalonate at 25 ℃-30 ℃ for 16 h. The yield of main products after condensation reached 74％ with 1.1/1/10/(3-4)mole ratio of monoethyl ester/ phosphonic aldehyde/ pyridine/anhydride. Finally,the structures of the product,2-acetamido-4-[hydroxy(methyl)phosphonyl]but-2-enoic acid was characterized by 1H, 13C and 31P nuclear magnetic resonance spectroscopy. Its total yield of intermediate is 63.1％ under the optimum reaction conditions. This synthetic route is suitable in industry production with simple operation and mild conditions.关键词
乙酰氨基丙二酸二乙酯/水解/缩合/2-乙酰氨基-4-[羟基(甲基)膦酰基]丁-2-烯酸/草铵膦Key words
diethyl acetamidomalonate/hydrolysis/condensation/2-acetylamino-4- [hydroxy (methyl) phosphonyl]but-2-enoic acid/glufosinate-ammonium分类
化学化工引用本文复制引用
吴忆雯,马银,冯薇伟,舒畅,奚强,户业丽,程波..一种草铵膦新型中间体的合成和表征[J].武汉工程大学学报,2018,40(1):17-22,6.基金项目
湖北省自然科学基金(2012FFB04704) （2012FFB04704）
