Réaction #1121556

ord-75d7e73e7d4d4b9ea4c190399871c09d

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autreat 80° C.
  2. 2
    Autreat 25° C., HP(=O)Et(OEt), or HP(=O)(OEt)2, a very exothermic reaction

Mode opératoire

It appears however that the HI3 salts of the monomethylenesulfonic acids of [9]aneN3 and [12]aneN3 can be used directly. When these triiodide 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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05316757uspto-grants-1994_05