Chlorosulfonic acid → 3,5-Dichloro-2,4,6-trifluorophenylsulfonyl chloride
Reaction equation
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([Cl:10])[C:3]=1[F:11].[Cl:12][S:13](O)(=[O:15])=[O:14]>>[Cl:1][C:2]1[C:7]([F:8])=[C:6]([S:13]([Cl:12])(=[O:15])=[O:14])[C:5]([F:9])=[C:4]([Cl:10])[C:3]=1[F:11]Participants
3
Conditions
- Temperature
- 80 °C
Procedure
1,3-Dichloro-2,4,6-trifluorobenzene (5.0 g, 25 mmol) and chlorosulfonic acid (10.0 ml, 150 mmol) were mixed at ambient temperature under a nitrogen atmosphere and the reaction was heated at 80° C. for 24 h. The mixture was then allowed to cool to ambient temperature and was poured onto 12 g of crushed ice. The product was extracted with diethyl ether, dried over MgSO4, and evaporated to produce 4.9 g of the title compound, which was used without further purification. MS (EI): 300 (30, M+), 298 (28), 263 (100), 199 (80).
Workup
- temperatureto cool to ambient temperature
- extractionThe product was extracted with diethyl ether
- dry with materialdried over MgSO4
- customevaporated
Sources & evidence
- ORD record
- ord-3e9ceaf8d7294a369721090362fe6c7c
- Source dataset
- uspto-grants-2001_09
- Patent number
- US06284923B1
Reaction notes
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