2,6-Difluorobenzoyl isocyanate → 3-[3,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)phenyl]-6-(2,6-difluorophenyl)-3,4-dihydro-2H-1,3,5-oxadiazine-2,4-dione

HRID 2290715Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2290715
[F:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:3]=1[C:4]([N:6]=[C:7]=[O:8])=[O:5].[Cl:14][C:15]1[CH:16]=[C:17]([N:29]=[C:30]=[O:31])[CH:18]=[C:19]([Cl:28])[C:20]=1[O:21][C:22]([F:27])([F:26])[CH:23]([F:25])[F:24]>>[Cl:14][C:15]1[CH:16]=[C:17]([N:29]2[C:7](=[O:8])[N:6]=[C:4]([C:3]3[C:2]([F:1])=[CH:12][CH:11]=[CH:10][C:9]=3[F:13])[O:5][C:30]2=[O:31])[CH:18]=[C:19]([Cl:28])[C:20]=1[O:21][C:22]([F:26])([F:27])[CH:23]([F:24])[F:25]

Komponenten

3

Edukt 2

HCID 27333692,6-Difluorobenzoyl isocyanateHCID 202301521,3-Dichloro-5-isocyanato-2-(1,1,2,2-tetrafluoroethoxy)benzene

Produkt 1

HCID 202301533-[3,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)phenyl]-6-(2,6-difluorophenyl)-3,4-dihydro-2H-1,3,5-oxadiazine-2,4-dione

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

With the exclusion of moisture, 5.4 g of 2,6-difluorobenzoylisocyanate are added with stirring to 9.1 g of 3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)phenylisocyanate. The temperature is maintained at 120° C. for 14 hours, with stirring being continued until the reaction mixture commences to congeal. When the resultant crystalline slurry has cooled to room temperature, it is triturated with hexane and subsequently filtered with suction. The residue is recrystallised from toluene, affording the title compound of the formula ##STR9## as a white powder with a melting point of 170°-172° C. (compound 1.2.1).

Aufarbeitung

  1. temperatureWhen the resultant crystalline slurry has cooled to room temperature
  2. customit is triturated with hexane
  3. filtrationsubsequently filtered with suction
  4. customThe residue is recrystallised from toluene

Quellen und Nachweise

ORD-Eintrag
ord-be56388a5d134fb8824adb17312d0b1d
Quelldatensatz
uspto-grants-1986_10
Patentnummer
US04618608

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