Reaktion #50742

Reaktionsgleichung

[9]aneN3

[12]aneN3

phosphorous acid

→

[9]aneN3

monomethylene(ethyl)-phosphinate ethyl ester

[12]aneN3

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONWhen these trilodide salts are added
2. 2
   Sonstigeat 80° C.
3. 3
   Sonstigeat 25° C., HP(=O)Et(OEt), or HP(=O)(OEt)2, a very exothermic reaction

Vorschrift

It appears however that the HI3 salts of the monomethylenesulfonic acids of [9]aneN3 and [12]aneN3 can be used directly. When these trilodide salts are added to melted phosphorous acid at 80° C., at 25° C., HP(=O)Et(OEt), or HP(=O)(OEt)2, a very exothermic reaction occurs whereby the respective monomethylenephosphonate, the monomethylene(ethyl)-phosphinate ethyl ester and the monomethylenephosphonate diethyl ester of [9]aneN3 (FIGS. 31A, 31B, and 31C) and the monomethylenephosphonate diethyl ester and the monomethylene(ethyl)-phosphinate ethyl ester of [12]aneN3 (FIGS. 32A and 32B) are formed almost quantitatively within a few seconds.

Quelle