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

HRID 1252086Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1252086
[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-61b2da111cef40618307e90a8308941d
Quelldatensatz
uspto-grants-1988_05
Patentnummer
US04742059

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