Hydrazine Sulfate → HCID 88768920, Verbindung

HRID 629201

Reaktionsgleichung

Reaktionsgleichung von HRID 629201
[Cl:1][C:2]1[C:7]2[C:8](=O)[O:9][CH:10](O)[C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1.S(O)(O)(=O)=O.[NH2:19][NH2:20].C([O-])(=O)C.[Na+]>O>[Cl:1][C:2]1[C:7]2[C:8](=[O:9])[NH:19][N:20]=[CH:10][C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1

Komponenten

5

Edukt 3

HCID 24842Hydrazine SulfateHCID 517045Sodium AcetateHCID 89972412HCID 89972412, Verbindung

Produkt 1

HCID 88768920HCID 88768920, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To a suspension of 4,6-dichloro-1-hydroxy-1H-furo[3,4-c]pyridin-3-one (9.37 g) stirring in water (100 ml) was added hydrazine sulfate (10.58 ml) and sodium acetate (13.56 g). The reaction mixture was heated at reflux and stirred for 2 h. The reaction mixture was cooled to RT, diluted with water (150 ml) and extracted with EtOAc (2×75 ml). The combined organic layers were washed with saturated Na2CO3 solution and dried over Na2SO4. Evaporation to dryness gave the desired product as brown solid.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux
  3. extractionextracted with EtOAc (2×75 ml)
  4. washThe combined organic layers were washed with saturated Na2CO3 solution
  5. dry with materialdried over Na2SO4
  6. customEvaporation to dryness

Quellen und Nachweise

ORD-Eintrag
ord-8c9942035d80453ba2ad8fdc7f24cb17
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09315500B2

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