Synthesis of Isotope labeled Trichlorfon-methoxyl-D6 and Dichlorophos-methoxyl-D6

• Main Author: YANG Wei-cheng1;LV Jing1;QI Qing-rui2;SHENG Li-yan1;LI Mei-hua1;YANG Chao1;LUO Yong1
• Format: Article
• Language: zho
• Published: Editorial Board of Journal of Isotopes 2014-02-01
• Series: Journal of Isotopes
• Subjects: isotope labeled synthesis dimethyl phosphate trichlorfon dichlorophos characterization
• Online Access: http://www.tws.org.cn/CN/10.7538/tws.2014.27.01.0008

The efficient synthesis of two labeled standards trichlorfon-methoxyl-D6 and dichlorophos- methoxyl-D6 with CD3OD as the precursor were presented. Esterification of phosphorus trichloride with CD3OD provided dimethyl phosphate-methoxyl-D6, which was used to condense with trichloroaldehyde to give trichlorfon-methoxyl-D6. Ttrichlorfon-methoxyl-D6 was further converted to dichlorophos-methoxyl-D6 by alkaline hydrolysis and rearrangement. The yields of trichlorfon-methoxyl-D6 and Dichlorophos-methoxyl-D6 were 57.7 % and 47.3% respectively based on CD3OD consumed. Both products were characterized by HPLC, MS, and NMR to be target compounds. Their chemical purities and isotopic enrichment were higher than 98.0%. The above compounds could be used as internal standards in the food safety field.