反应详情

To a solution of phenylhydrazine (4.5 g, 0.0423 mole) in 40 ml. of ether was added dropwise with good stirring ethyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate (3.3 g, 0.01 mole) dissolved in ether. The reaction was stirred at room temperature for two hours, then filtered and the filtrate concentrated in vacuo to give a gum-solid. This was triturated with petroleum ether, then ether. The ether insoluble solid was washed with water to give ethyl N-trifluoroacetyl-N-(bis(phenylhydrazino)phosphonomethyl)glycinate (0.6 g), m.p. 113°-116° C. (glass), 143°-145° C. with decomposition.

1. filtrationfiltered
2. concentrationthe filtrate concentrated in vacuo
3. customto give a gum-solid
4. customThis was triturated with petroleum ether
5. washThe ether insoluble solid was washed with water