Ethylene → Phosphinic acid, P,P-diethyl-, aluminum salt (3:1)

HRID 1868565

Reaction equation

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]

Participants

Conditions

Temperature: 100 °C

Procedure

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.

Workup

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.

Sources & evidence

ORD record: ord-feb51ac16d124481b93e8e32d6a1d416
Source dataset: uspto-grants-2009_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07635785B2

Linked notes

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