Sulfuric Acid → Bis(trifluoromethyl) disulfide
Reaction equation
[F:1][C:2]([S:5][S:6][C:7]([F:10])([F:9])[F:8])([F:4])[F:3].S(=O)(=O)(O)O.[Cl:16]Cl>>[F:1][C:2]([F:4])([F:3])[S:5][Cl:16].[F:1][C:2]([S:5][S:6][C:7]([F:10])([F:9])[F:8])([F:4])[F:3]Participants
5
Conditions
- Temperature
- 40 °C
Procedure
4,040 g of bis-(trifluoromethyl) -disulfane and 2,000 g of 96% strength sulfuric acid were initially placed in a 10 l Hasteloy autoclave and were charged at 18° C. with a pressure of 5 bar of nitrogen. 1,000 ml of liquid chlorine were pumped into this solution at 40° C. in the course of 2 hours. The reaction mixture was stirred for a further 12 hours at 40° C. and under a pressure of 14 to 16 bar, and it was then purified by distillation. 4,250 g of trifluoromethanesulfenyl chloride having a boiling point of 0° C. at normal pressure and 350 g of unreacted bis-(trifluoromethyl) -disulfane were obtained.
Workup
- additionwere charged at 18° C. with a pressure of 5 bar of nitrogen
- customwere pumped into this solution at 40° C. in the course of 2 hours
- distillationwas then purified by distillation
Sources & evidence
- ORD record
- ord-572a07266fa6420fbad3f7006a2282be
- Source dataset
- uspto-grants-1992_02
- Patent number
- US05087747
Reaction notes
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