Antimony pentachloride → HCID 67783068, 화합물

HRID 249406

반응식

HRID 249406 반응식
[F:1][C:2]1[N:7]=[C:6]([F:8])[N:5]=[C:4](OC(Cl)(Cl)Cl)[N:3]=1.[Sb](F)(F)F.[Sb](Cl)(Cl)(Cl)(Cl)[Cl:19].FC1N=C(F)N=C([O:32][C:33]([F:36])(F)[F:34])N=1>>[Cl:19][C:4]1[N:5]([O:32][CH:33]([F:36])[F:34])[CH:6]([F:8])[N:7]=[C:2]([F:1])[N:3]=1

참가 물질

5

반응물 4

HCID 24294Antimony pentachlorideHCID 24554Antimony trifluorideHCID 150103862,4-Difluoro-6-(trichloromethoxy)-1,3,5-triazineHCID 150103872,4-Difluoro-6-(trifluoromethoxy)-1,3,5-triazine

생성물 1

HCID 67783068HCID 67783068, 화합물

반응 조건

온도
110 °C

실험 절차

210 g (0.838 mol) of 2,4-difluoro-6-trichloromethoxy-1,3,5-triazine were added within 10 minutes to 110 g (0.615 mol) of antimony trifluoride while stirring at 110° C. After addition of 3/4 of 9.38 g (0.0313 mol) of antimony pentachloride, the mixture was heated to 145° C. and stirred for 1 hour. The remaining catalyst was added, and the mixture was stirred for a further 2 hours while a fraction boiling at 95°-105° C. was obtained through a 30 cm packed column: 20 g (11.8% of theory) of 2,4-difluoro-6-trifluoromethoxy-1,3,5-triazine. The residue was distilled without a column to yield 94.8 g (52% of theory) of the title compound of boiling point 125°-130° C.; nD24 =1.4042.

후처리

  1. temperaturethe mixture was heated to 145° C.
  2. stirringstirred for 1 hour
  3. additionThe remaining catalyst was added
  4. stirringthe mixture was stirred for a further 2 hours while a fraction boiling at 95°-105° C.
  5. customwas obtained through a 30 cm
  6. distillationThe residue was distilled without a column

출처 및 근거

ORD 기록
ord-05182873159749ab80ee1bc4adfcc02f
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05214143

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