Quintozene → 1,2-Dichloro-3-fluoro-4-nitrobenzene

HRID 988003

Reaktionsgleichung

Reaktionsgleichung von HRID 988003
ClC1C([N+]([O-])=O)=C(Cl)C(Cl)=C(Cl)C=1Cl.ClC1C([N+]([O-])=O)=C(F)C(F)=C(F)C=1Cl.ClC1C([N+]([O-])=O)=C(F)C(F)=C(Cl)C=1Cl.Cl[C:44]1[C:49]([N+:50]([O-:52])=[O:51])=[C:48]([F:53])[C:47]([Cl:54])=[C:46]([Cl:55])[C:45]=1Cl>C(#N)C>[Cl:55][C:46]1[CH:45]=[CH:44][C:49]([N+:50]([O-:52])=[O:51])=[C:48]([F:53])[C:47]=1[Cl:54]

Komponenten

6

Edukt 4

HCID 6720QuintozeneHCID 13099723HCID 13099723, Verbindung2×HCID 22987219DichlorotrifluoronitrobenzeneHCID 22987224Trichloro-difluoronitrobenzene2×

Produkt 1

HCID 229872151,2-Dichloro-3-fluoro-4-nitrobenzeneAusbeute 28 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a reaction vessel, 0.74 g(2.50 m mol) of pentachloronitrobenzene, 1.77 g (13.00 m mol) of DFI, and 25 ml of acetonitrile were charged and reacted at 84° C. for 2 hours in a nitrogen atmosphere. After finishing the reaction, formation of dichlorotrifluoronitrobenzene (master ion, 245, master ion +2 247, master ion +4 249, base peak 245) was confirmed by GC-MS measurement on the reaction mixture, and the yield was 28.0% by GC analysis. Formation of trichloro-difluoronitrobenzene (master ion 261, master ion +2 263, master ion +4 265, base peak 205) was also confirmed and the yield was 11.3%. Formation of tetrachlorofluoronitrobenzene (master ion 277, master ion+2 279, master ion+4 281, master ion+6 283, base peak 221) was further confirmed and the yield was 9.0%.

Aufarbeitung

  1. customreacted at 84° C. for 2 hours in a nitrogen atmosphere

Quellen und Nachweise

ORD-Eintrag
ord-b1e0f89d96b44a378ff0b1f043d741d7
Quelldatensatz
uspto-grants-2003_10
Patentnummer
US06632949B2

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