Hydrazine → HCID 178518904, Verbindung

HRID 2357513Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2357513
C([N:5]1[CH:13](O)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:15])[CH:11]=2)[C:6]1=[O:16])(C)(C)C.[NH2:17]N>C(O)(=O)C>[Cl:15][C:10]1[CH:11]=[C:12]2[C:7](=[CH:8][CH:9]=1)[C:6]([OH:16])=[N:17][N:5]=[CH:13]2

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 251930612-Tert-butyl-5-chloro-3-hydroxyisoindolin-1-one

Produkt 1

HCID 178518904HCID 178518904, VerbindungAusbeute 98,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A suspension of 2-tert-butyl-5-chloro-3-hydroxyisoindolin-1-one (5.26 g, 21.9 mmol) in glacial acetic acid (32 mL) was heated with stirring until the mixture became a clear solution. Anhydrous hydrazine (1.0 mL, 22 mmol) was added dropwise and the resultant solution was stirred at reflux overnight. The reaction mixture was concentrated under reduced pressure. Water was added to the mixture, after which a solid material precipitated out of the solution. The solid was collected by filtration and rinsed thoroughly with water, followed by air-drying to afford 6-chlorophthalazin-1-ol (3.9 g, 98% yield) as an off-white powder (mp 271-273° C.).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionWater was added to the mixture
  5. customafter which a solid material precipitated out of the solution
  6. filtrationThe solid was collected by filtration
  7. washrinsed thoroughly with water
  8. customby air-drying

Quellen und Nachweise

ORD-Eintrag
ord-1cc79bce83f54b89a8aef1d1ae90c871
Quelldatensatz
uspto-grants-2010_07
Patentnummer
US07759337B2

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