Monobasic potassium phosphate → 5,8-Dihydroquinoline-5,8-dione

HRID 2308947Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2308947
[OH:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.P([O-])(O)(O)=[O:13].[K+].N(S([O-])(=O)=O)(S([O-])(=O)=O)[O].[K+].[K+]>CO.O>[N:7]1[C:8]2[C:9](=[O:13])[CH:10]=[CH:11][C:2](=[O:1])[C:3]=2[CH:4]=[CH:5][CH:6]=1

Komponenten

6

Edukt 3

HCID 516951Monobasic potassium phosphateHCID 3032624Potassium nitrosodisulfonateHCID 135441757Quinolin-5-ol

Produkt 1

HCID 3883065,8-Dihydroquinoline-5,8-dioneAusbeute 47,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 23.2 g of 5-hydroxyquinoline in 1600 ml of methanol in an ice bath was added a total of 36 g of potassium dihydrogen phosphate and 96 g of potassium nitroso disulfonate in 8.8 liters of water in five portions over a 1 hour period. The mixture was then stirred overnight at room temperature, followed by extraction with four 1500 ml portions of chloroform. The extracts were combined, dried, filtered through alumina and evaporated to dryness, giving 12.0 g of crude product. An analytical sample was prepared by crystallization from petroleum ether, mp 110° C.

Aufarbeitung

  1. extractionfollowed by extraction with four 1500 ml portions of chloroform
  2. customdried
  3. filtrationfiltered through alumina
  4. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-ad7559ae3c4144d18cc6537b4e9b745b
Quelldatensatz
uspto-grants-1987_09
Patentnummer
US04692449

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