Reaktionsgleichung
O.[PH2:2]([O-:4])=[O:3].[Na+].[CH2:6]=[CH2:7].Cl.N([C:17]([C:20](=N)N)(C)C)=N[C:11](C(=N)N)(C)[CH3:12].O.O.O.O.O.O.[Cl-].[Al+3:30].[Cl-].[Cl-]>O>[CH2:11]([P:2]([CH2:6][CH3:7])(=[O:4])[O-:3])[CH3:12].[Al+3:30].[CH2:6]([P:2]([CH2:17][CH3:20])(=[O:4])[O-:3])[CH3:7].[CH2:11]([P:2]([CH2:6][CH3:7])(=[O:4])[O-:3])[CH3:12]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
1500 g (14 mol) of sodium hypophosphite monohydrate were dissolved in 7.5 kg of water and used as initial charge in a 16 l jacketed pressure reactor composed of enameled steel. Once the reaction mixture had been heated to 100° C., ethylene was introduced by way of a reducing valve set to 6 bar until saturation had been reached in the reactor. A solution of 19 g (0.5 mol %) of 2,2′-azobis(2-amidinopropane) hydrochloride (Wako Pure Chemical Industries, Ltd., grade V50 98.8%) in 300 g of water was uniformly metered in over a period of 6 h with constant stirring, at an ethylene pressure of 6 bar and a temperature of from 100 to 110° C. After a continued reaction time of 1 h, depressurization of the reactor, and cooling to about 90° C., 650 g (4.67 mol of aluminum) of aluminum chloride hexahydrate in 2350 g of water were added over a period of 60 min. The resultant solid was then filtered off, washed with 2 l of hot water and vacuum-dried at 130° C.
Aufarbeitung
- additionas initial charge in a 16 l jacketed pressure reactor
- customof from 100 to 110° C
- temperatureAfter a continued reaction time of 1 h, depressurization of the reactor, and cooling to about 90° C.
- filtrationThe resultant solid was then filtered off
- washwashed with 2 l of hot water
- customvacuum-dried at 130° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-feb51ac16d124481b93e8e32d6a1d416
- Quelldatensatz
- uspto-grants-2009_12
- Patentnummer
- US07635785B2
Verknüpfte Notizen
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