同位素标记敌百虫-甲氧基-D6和敌敌畏-甲氧基-D6的合成

以CD30D为同位素源，经与三氯化磷酯化得到亚磷酸二甲酯，再进一步与三氯乙醛加成得到敌百虫-甲氧基-D6，碱解脱去氯化氢分子，重排后生成敌敌畏-甲氧基-D-6.以消耗CD3OD计算稳定同位素标记敌百虫-甲氧基-D6和敌敌畏-甲氧基-D6提纯后总收率分别为57．7％和47．3％。产物经高效液相色谱（HPLC）、质谱（MS）和核磁（NMR）等仪器的鉴定为目标物质，化学纯度大于98．0％，同位素丰度高于98．0％，可作为食品安全领域检测用同位素内标试剂。...

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Bibliographic Details
Published in同位素 Vol. 27; no. 1; pp. 8 - 14
Main Author 杨维成 吕靖 齐庆瑞 盛立彦 李美华 杨超 罗勇
Format Journal Article
LanguageChinese
Published 上海化工研究院技术开发中心上海200062%新疆教育学院职业教育分院,乌鲁木齐,830046 2014
Subjects
合成
同位素标记
敌敌畏
敌百虫
表征
synthesis
合成
敌百虫
isotope labeled
trichlorfon dichlorophos
同位素标记
敌敌畏
表征
dimethyl phosphite
characterization
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Summary:以CD30D为同位素源，经与三氯化磷酯化得到亚磷酸二甲酯，再进一步与三氯乙醛加成得到敌百虫-甲氧基-D6，碱解脱去氯化氢分子，重排后生成敌敌畏-甲氧基-D-6.以消耗CD3OD计算稳定同位素标记敌百虫-甲氧基-D6和敌敌畏-甲氧基-D6提纯后总收率分别为57．7％和47．3％。产物经高效液相色谱（HPLC）、质谱（MS）和核磁（NMR）等仪器的鉴定为目标物质，化学纯度大于98．0％，同位素丰度高于98．0％，可作为食品安全领域检测用同位素内标试剂。
Bibliography:11-2566/TL
isotope labeled; synthesis; dimethyl phosphite; trichlorfon dichlorophos ; char-acterization
YANG Wei-cheng , LV Jing , QI Qing-rui , SHENG Li-yan , LI Mei-hua , YANG Chao , LUO Yong （1. R ＆ D Center, Shanghai Research Institute of Chemical Industry ,Shanghai 200062, China ; 2. Branch of Professional Education, Xinjiang Education Institute, Urumqi 830046, China）
The efficient synthesis of two labeled standards trichlorfon-methoxyl-D6 and di- ehlorophos- methoxyl-D6 with CD3OD as the precursor were presented. Esterification of phosphorus trichloride with CD3OD provided dimethyl phosphite-methoxyl-D6, which was used to condense with trichloroaldehyde to give triehlorfon-methoxyl-D6. Ttrichlorfon-me- thoxyl-D6 was further converted to dichlorophosvmethoxyl-D6 by alkaline hydrolysis and re- arrangement. The yields of trichlorfon-methoxyl-D6 and Dichlorophos-methoxyl-D6 were 57.7 % and 47.3% respectively based on CD3OD consumed. Both products were character- ized by HPLC, MS, and NMR to be target compounds
ISSN:1000-7512
DOI:10.7538/tws.2014.27.01.0008