Synthesis of Isotope labeled Trichlorfon-methoxyl-D_6 and Dichlorophos-methoxyl-D_6
2014
The efficient synthesis of two labeled standards trichlorfon-methoxyl-D6and dichlorophos-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 trichlorfon-methoxyl-D6.Ttrichlorfon-methoxyl-D6 was further converted to dichlorophos-methoxyl-D6by 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 isotopicenrichment were higher than 98.0%.The above compounds could be used as internal standards in the food safety field.
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