Phosphorous acid → 1,4,7-Triazacyclononane

HRID 22464

Reaktionsgleichung

Reaktionsgleichung von HRID 22464
[CH2:1]1[NH:9][CH2:8][CH2:7][NH:6][CH2:5][CH2:4][NH:3][CH2:2]1.[CH2:10]1[CH2:21][NH:20][CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14][CH2:13][NH:12][CH2:11]1.[P:22](O)([OH:24])[OH:23]>>[CH2:1]1[NH:9][CH2:8][CH2:7][NH:6][CH2:5][CH2:4][NH:3][CH2:2]1.[CH2:7]([O:24][PH:22]([CH2:19][CH:18]=[CH2:17])=[O:23])[CH3:8].[CH2:18]1[CH2:17][NH:16][CH2:15][CH2:14][CH2:13][NH:12][CH2:11][CH2:10][CH2:21][NH:20][CH2:19]1

Komponenten

6

Edukt 3

HCID 107909Phosphorous acidHCID 1883181,4,7-TriazacyclononaneHCID 4707781,5,9-Triazacyclododecane

Produkt 3

HCID 1883181,4,7-TriazacyclononaneHCID 4707781,5,9-TriazacyclododecaneHCID 178460680HCID 178460680, Verbindung

Versuchsvorschrift

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.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-c7dec6c7de3e4f5bbe8bd04851220980
Quelldatensatz
uspto-grants-1995_06
Patentnummer
US05428155

Verknüpfte Notizen

Wird geladen…