Hydrogen Bromide → p,p'-(Phenylphosphinylidene)bisphenol

HRID 1270561

Reaktionsgleichung

Reaktionsgleichung von HRID 1270561
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([P:9](=[O:24])([C:16]2[CH:21]=[CH:20][C:19]([O:22]C)=[CH:18][CH:17]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.Br.[Br-].[K+].S([O-])([O-])=O.[Na+].[Na+].CBr>>[OH:2][C:3]1[CH:8]=[CH:7][C:6]([P:9](=[O:24])([C:16]2[CH:17]=[CH:18][C:19]([OH:22])=[CH:20][CH:21]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1

Komponenten

6

Edukt 5

HCID 260Hydrogen BromideHCID 6323Methyl BromideHCID 24437Sodium SulfiteHCID 253877Potassium BromideHCID 4589182Bis(4-methoxyphenyl)phenylphosphine oxide

Produkt 1

HCID 69930p,p'-(Phenylphosphinylidene)bisphenolAusbeute 74 %

Versuchsvorschrift

Bis(4-methoxyphenyl)phenylphosphine oxide mixture (2359 g, 6.97 mol), hydrobromic acid (48%, 8344 g, 49.5 mol), and potassium bromide (243 g, 2.04 mol) were stirred at 120° C. for 48 h. The flask was fitted with a sodium sulfite scrubber for containment of methyl bromide. The lower aqueous layer was removed and the product layer was worked up to afford bis(4-hydroxyphenyl)phenylphosphine oxide mixture (Composition VI) as a tan powder (1601 g, 74%). m.p. (DSC): 93° C. 31P NMR (d6-DMSO): δ 27.7 (s, 24.7%); 27.5 (s, 47.7%); 27.4 (s, 25.4%); 27.2 (s, 2.2%).

Aufarbeitung

  1. customThe lower aqueous layer was removed

Quellen und Nachweise

ORD-Eintrag
ord-d7bac0f34a684f858a5e1936117b0a03
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07202311B2

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