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Nucleophilic amination of chloromethylphosphonic esters was studied. α-Dideuteriated aminomethyl-phosphonic acid was obtained from bis(trifluoroethyl) chloromethylphosphonic ester and sodium azide through substitution of the chlorine, reduction of the azide and acidic hydrolysis. Incorporation of the deuterium was greater than 95% and overall yields were in the range 55–65%.
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