METHYL-2-N-(ACETYLAMINO)-DIMETHYL PHOSPHONO ACETATE

108-24-7

100945-15-1

89524-99-2

GENERAL STEPS: Compound C152 (12.65 g, 38.2 mmol) and acetic anhydride (9.02 mL, 95.5 mmol) were dissolved in methanol (100 mL), and the mixed solution was transferred to a Parr autoclave. 10% Pd/C catalyst (0.640 g) was added and the hydrogenation reaction was carried out at 45 psi hydrogen pressure for 3 hours. Upon completion of the reaction, the catalyst was removed by filtration and the filtrate was concentrated under reduced pressure to give an oil. The oil was placed in a depressurized environment and reduced pressure was applied to solidify it. The resulting white solid was dissolved in a small amount of ethyl acetate and pentane was slowly added with vigorous stirring until a precipitate began to form. The precipitate was separated by filtration to give methyl 2-acetamido-2-(dimethoxyphosphoryl)acetate (C153) as a white powder in 87% yield. Mass spectrometry (chemical ionization, CI) analysis showed a molecular ion peak (M+H)+ m/z of 240 for C7H14NO6P.