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 2290715노트

반응식

HRID 2290715 반응식
[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]

참가 물질

3

반응물 2

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

생성물 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

반응 조건

온도
120 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-be56388a5d134fb8824adb17312d0b1d
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04618608

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