Sulfite → 1,4,5,8-Naphthalenetetracarboxylic acid

HRID 1656855

Reaktionsgleichung

Reaktionsgleichung von HRID 1656855
ClCl.BrBr.S([O-])([O-])=O.C1C(C(N)=O)=CN(C2OC(COP(OP(OCC3OC(N4C5N=CN=C(N)C=5N=C4)C(OP([O-])([O-])=O)C3O)([O-])=O)([O-])=O)C(O)C2O)C=C1.[Na+:57].[Na+:58].[Na+].[Na+].[C:61]1([C:80]([OH:82])=[O:81])[C:70]2[C:69]([C:71]([OH:73])=[O:72])=[CH:68][CH:67]=[C:66]([C:74]([OH:76])=[O:75])[C:65]=2[C:64]([C:77]([OH:79])=[O:78])=[CH:63][CH:62]=1>>[Na:57][Na:58].[C:61]1([C:80]([OH:82])=[O:81])[C:70]2[C:69]([C:71]([OH:73])=[O:72])=[CH:68][CH:67]=[C:66]([C:74]([OH:76])=[O:75])[C:65]=2[C:64]([C:77]([OH:79])=[O:78])=[CH:63][CH:62]=1

Komponenten

7

Edukt 5

HCID 1099SulfiteHCID 24408BromineHCID 24526ChlorineHCID 314221,4,5,8-Naphthalenetetracarboxylic acidHCID 12598259[2-adenin-9-yl-5-[[[[5-(3-carbamoyl-4H-pyridin-1-yl)-3,4-dihydroxy-tetrahydrofuran-2-yl]methoxy-oxido-phosphoryl]oxy-oxido-phosphoryl]oxymethyl]-4-hydroxy-tetrahydrofuran-3-yl] phosphate

Produkt 2

HCID 314221,4,5,8-Naphthalenetetracarboxylic acidHCID 141233Disodium

Versuchsvorschrift

In the aqueous-alkaline hypohalite oxidation of organic compounds, in particular in the alkaline hypochlorite oxidation of 2,7-dibromodiindanedione (3) to give the tetraalkali metal salt of naphthalene-1,4,5,8-tetracarboxylic acid, the ecological pollution by halogen-containing compounds of the classes CHX3 and CX4, in which X is chlorine, bromine or a combination thereof, is eliminated by carrying out the aqueous-alkaline hypohalite oxidation at a temperature of between 20° and 60° C., preferably 40° to 55° C., in a closed vessel under the autogenous pressure which is established at the corresponding temperature, subjecting the reaction mixture, after the oxidation has ended, to a heat treatment at a temperature of between 90° and 120° C., preferably 90° to 100° C., under the autogenous pressure of 1 to 10 bar, preferably 1 to 5 bar, which is established, in the presence of sulfite, cooling the resulting suspension of the tetrasodium salt of naphthalene-1,4,5,8-tetracarboxylic acid, after the reaction vessel has been let down, to a temperature of below 40° C., preferably to 20° to 30° C., subsequently adjusting the pH to 4.5 to 5 by acidification, isolating the resulting disodium salt of naphthalene-1,4,5,8-tetracarboxylic acid, converting this salt into the tetrasodium salt of naphthalene-1,4,5,8-tetracarboxylic acid in an aqueous alkali metal hydroxide solution and, if appropriate after removal of insoluble impurities, precipitating naphthalene-1,4,5,8-tetracarboxylic acid 1,8-monoanhydride by acidification to a pH of less than 2, preferably less than 1, at a temperature of 80° to 100° C.

Aufarbeitung

  1. customat a temperature of between 20° and 60° C., preferably 40° to 55° C.
  2. customin a closed vessel under the autogenous pressure which is established at the corresponding temperature
  3. customhas ended, to a heat treatment at a temperature of between 90° and 120° C., preferably 90° to 100° C., under the autogenous pressure of 1 to 10 bar, preferably 1 to 5 bar, which
  4. temperaturecooling
  5. customhas been let down, to a temperature of below 40° C., preferably to 20° to 30° C.

Quellen und Nachweise

ORD-Eintrag
ord-549f37eecbc5416b837f8947a2e457b3
Quelldatensatz
uspto-grants-1993_10
Patentnummer
US05254796

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