Reaction equation
[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]=1Participants
5
Conditions
- Temperature
- 110 °C
Procedure
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.
Workup
- temperaturethe mixture was heated to 145° C.
- stirringstirred for 1 hour
- additionThe remaining catalyst was added
- stirringthe mixture was stirred for a further 2 hours while a fraction boiling at 95°-105° C.
- customwas obtained through a 30 cm
- distillationThe residue was distilled without a column
Sources & evidence
- ORD record
- ord-05182873159749ab80ee1bc4adfcc02f
- Source dataset
- uspto-grants-1993_05
- Patent number
- US05214143
Linked notes
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