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 2290715ノート

反応式

HRID 2290715 の反応式
[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]

参加物

3

反応物 2

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

生成物 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

反応条件

温度
120 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-be56388a5d134fb8824adb17312d0b1d
出典データセット
uspto-grants-1986_10
特許番号
US04618608

反応ノート

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