Sodium Sulfate → 4-(Pentafluorophenyl)-1,2,4-triazoline-3,5-dione

HRID 1902896Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1902896
[F:1][C:2]1[C:7]([N:8]2[C:12](=[O:13])[NH:11][NH:10][C:9]2=[O:14])=[C:6]([F:15])[C:5]([F:16])=[C:4]([F:17])[C:3]=1[F:18].S([O-])([O-])(=O)=O.[Na+].[Na+]>C(OCC)(=O)C>[F:15][C:6]1[C:7]([N:8]2[C:9](=[O:14])[N:10]=[N:11][C:12]2=[O:13])=[C:2]([F:1])[C:3]([F:18])=[C:4]([F:17])[C:5]=1[F:16]

Komponenten

4

Edukt 2

HCID 24436Sodium SulfateHCID 129043794-(Pentafluorophenyl)urazole

Produkt 1

HCID 129043834-(Pentafluorophenyl)-1,2,4-triazoline-3,5-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A 50 ml, three-necked flask is fitted with a gas-dispersion tube, a drying tube and a stirrer. 4-(Pentafluorophenyl)urazole, 0.5 g (1.8 mM) is dissolved in 25 ml of ethyl acetate. Anhydrous sodium sulfate, 3 g, is added to remove water present in NO2. The reaction mixture is cooled in an ice bath, and nitrogen dioxide added slowly for 20 minutes. The mixture is allowed to stir for 20 minutes. The Na2SO4 is removed by filtration and the ethyl acetate removed with the rotary evaporator to yield a red oil. The residual solvent is removed with a vacuum pump to yield a crystalline solid, 0.35 g, mp 88°-91° C. The product is further purified by sublimation, mp 94°-96° C.

Aufarbeitung

  1. customA 50 ml, three-necked flask is fitted with a gas-dispersion tube, a drying tube and a stirrer
  2. customto remove water
  3. temperatureThe reaction mixture is cooled in an ice bath
  4. additionnitrogen dioxide added slowly for 20 minutes
  5. customThe Na2SO4 is removed by filtration
  6. customthe ethyl acetate removed with the rotary evaporator
  7. customto yield a red oil
  8. customThe residual solvent is removed with a vacuum pump
  9. customto yield a crystalline solid, 0.35 g, mp 88°-91° C
  10. customThe product is further purified by sublimation, mp 94°-96° C.

Quellen und Nachweise

ORD-Eintrag
ord-2b0fa37bf6af4c12bd1c9bb8c74e4ee2
Quelldatensatz
uspto-grants-1982_12
Patentnummer
US04366320

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