Reaktion #47179

Reaktionsgleichung

1,10-phenanthroline-5,6-dione

dithioxamide

→

5,6-dihydroxy-1,10-phenanthroline

Ausbeute 75.2%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder heating in an atmosphere of air for 13 hours
2. 2
   SonstigeThe resultant reaction mixture
3. 3
   Filtrationsubjected to a suction filtration
4. 4
   Sonstigeobtaining powders
5. 5
   SonstigeFor removing substances
6. 6
   Waschenthe powders were washed with 100 ml of chloroform at room temperature
7. 7
   Filtrationfollowed by a suction filtration

Vorschrift

1 g of 1,10-phenanthroline-5,6-dione (reagent; manufactured and sold by Sigma-Aldrich Co., U.S.A.) and 0.691 g of dithioxamide (reagent; manufactured and sold by Tokyo Kasei Kogyo Co., Ltd., Japan) were added to 40 ml of ethanol, and the resultant mixture was refluxed under heating in an atmosphere of air for 13 hours. The resultant reaction mixture was allowed to cool to room temperature, and subjected to a suction filtration using a filter paper (pore diameter: 1 μm), thereby obtaining powders. For removing substances remaining unreacted in the obtained powders, the powders were washed with 100 ml of chloroform at room temperature while stirring, followed by a suction filtration using a filter paper (pore diameter: 1 μm), thereby obtaining 0.759 g of 5,6-dihydroxy-1,10-phenanthroline in the form of powders.

Quelle