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

HRID 911114Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 911114
[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. MS m/z=199 [M+1]+. Calc'd for C8H4F2N2O2: 198.13.

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-f66f15f5569e4c5aaa8db06d03b420e4
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08022221B2

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