同位素标记敌百虫-甲氧基-D_6和敌敌畏-甲氧基-D_6的合成

Synthesis of Isotope labeled Trichlorfon-methoxyl-D_6 and Dichlorophos-methoxyl-D_6

以CD3OD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-D6。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。

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. Their chemical purities and isotopicenrichment were higher than 98.0%. The above compounds could be used as internal stand- ards in the food safety field.