1,4,5,8-Naphthalenetetracarboxylic acid → 1,3-Dioxo-1H,3H-naphtho(1,8-cd)pyran-6,7-dicarboxylic acid

HRID 1656857

Reaktionsgleichung

Reaktionsgleichung von HRID 1656857
[C:1]1([C:20]([OH:22])=[O:21])[C:10]2[C:9]([C:11]([OH:13])=[O:12])=[CH:8][CH:7]=[C:6]([C:14]([OH:16])=[O:15])[C:5]=2[C:4]([C:17]([OH:19])=O)=[CH:3][CH:2]=1.[Na][Na]>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+].[Na+].[Na+].[Na+]>[C:6]12[C:14](=[O:16])[O:15][C:17](=[O:19])[C:4]3[C:5]1=[C:10]([C:1]([C:20]([OH:22])=[O:21])=[CH:2][CH:3]=3)[C:9]([C:11]([OH:13])=[O:12])=[CH:8][CH:7]=2

Komponenten

5

Edukt 2

HCID 314221,4,5,8-Naphthalenetetracarboxylic acid2×HCID 141233Disodium

Produkt 1

HCID 1323361,3-Dioxo-1H,3H-naphtho(1,8-cd)pyran-6,7-dicarboxylic acidAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 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] phosphateLösungsmittel2×

Versuchsvorschrift

After cooling to a temperature of 20° to 30° C., the suspension, which was present after the letting down, of the tetrasodium salt of naphthalene-1,4,5,8-tetracarboxylic acid (NTC) was worked up by a process analogous to that described in Example 3 c) , by a procedure in which the disodium salt of NTC was first formed by acidification to pH 4.8 to 4.5 and was isolated, this salt was then dissolved in water by conversion into the tetrasodium salt, insoluble impurities were separated off by filtration, and the 1,8-monoanhydride of NTC was then precipitated by acidification with hydrochloric acid and was isolated. 13.1 kg of naphthalene-1,4,5,8-tetracarboxylic acid 1,8-monoanhydride of 96% purity, corresponding to a yield of 97% of theory, were obtained.

Aufarbeitung

  1. temperatureAfter cooling to a temperature of 20° to 30° C.
  2. customwas first formed by acidification to pH 4.8 to 4.5
  3. customwas isolated
  4. customwere separated off by filtration
  5. customthe 1,8-monoanhydride of NTC was then precipitated by acidification with hydrochloric acid
  6. customwas isolated

Quellen und Nachweise

ORD-Eintrag
ord-20723f5bb0344f3383d0149c69f6c215
Quelldatensatz
uspto-grants-1993_10
Patentnummer
US05254796

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