Acetic Acid → 5,8-Difluoro-2,3-dihydrophthalazine-1,4-dione

HRID 227754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 227754
[F:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[C:7]2[C:3]=1[C:4](=O)[O:5][C:6]2=[O:12].C([O-])(=O)C.[Na+].C(O)(=O)C.[NH2:23][NH2:24]>O>[F:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[C:7]2[C:3]=1[C:4](=[O:5])[NH:23][NH:24][C:6]2=[O:12]

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 9321HydrazineHCID 5139183,6-Difluorophthalic anhydrideHCID 517045Sodium Acetate

Produkt 1

HCID 667320095,8-Difluoro-2,3-dihydrophthalazine-1,4-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 4,7-difluoroisobenzofuran-1,3-dione (1.00 g, 5.43 mmol) and sodium acetate (0.535 g, 6.52 mmol) was added water (14 mL), acetic acid (7.15 ml, 125 mmol) and hydrazine (0.205 ml, 6.52 mmol)(slowly). A water condenser was attached and the mixture was heated to reflux for 20 hours. Cooled to RT and filtered the resulting solid. Washed with water and dried to yield 5,8-difluoro-2,3-dihydrophthalazine-1,4-dione as a white solid.

Aufarbeitung

  1. customA water condenser was attached
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 20 hours
  4. filtrationfiltered the resulting solid
  5. washWashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-5460c3ba3c4a4c8fa56cd25eccb4a0ca
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07560551B2

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