반응 #1166454

반응 방정식

glyoxylic acid

aminomethanephosphonic acid

→

N-phosphonomethylglycine

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONAfter completion of the addition
2. 2
   workup.STIRRINGThe mixture was stirred for a further 15 min at 85° C.
3. 3
   온도the mixture was cooled

실험 절차

29.6 g (0.2 mol) of 50% strength aqueous glyoxylic acid solution were warmed to 40° C. with stirring. 11.1 g (0.1 mol) of aminomethanephosphonic acid were then added in portions at 40°-45° C., whereupon a vigorous evolution of gas commenced. After completion of the addition, the temperature was increased to an internal temperature of 85° C. After about 1 h, the evolution of gas was complete. The mixture was stirred for a further 15 min at 85° C., a little water was added, and the mixture was cooled. 10 g N-phosphonomethylglycine, m.p.: 321°-323° C. [decomp.], were obtained. After concentration of the mother liquor and digestion of the precipitated crystal slurry using methanol/water, a further 2.5 g was obtained. The total yield was thus 74% of theory.

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