Chlorosulfonic acid → HCID 21482735, compound
Reaction equation
[NH2:1][C:2]1[C:7]([Br:8])=[CH:6][C:5]([S:9](N)(=[O:11])=[O:10])=[CH:4][C:3]=1[Br:13].[Cl:14]S(O)(=O)=O>>[NH2:1][C:2]1[C:7]([Br:8])=[CH:6][C:5]([S:9]([Cl:14])(=[O:11])=[O:10])=[CH:4][C:3]=1[Br:13]Participants
3
Procedure
A solution of 15 g. of 4-amino-3,5-dibromobenzenesulfonamide in 45 ml. of chlorosulfonic acid is heated on a steam bath at 95° C. for 2 hours. The reaction mixture is cooled and poured onto 400 ml. of ice/water mixture. The resultant precipitate is filtered, dissolved in methylene chloride, and the methylene chloride solution is dried, filtered and evaporated to dryness, affording 4-amino-3,5-dibromobenzenesulfonylchloride, m.p. 153°-155° C.
Workup
- temperatureThe reaction mixture is cooled
- additionpoured onto 400 ml
- filtrationThe resultant precipitate is filtered
- dissolutiondissolved in methylene chloride
- dry with materialthe methylene chloride solution is dried
- filtrationfiltered
- customevaporated to dryness
Sources & evidence
- ORD record
- ord-049d1f0fd1c8402a8c8165f8f529268e
- Source dataset
- uspto-grants-1977_01
- Patent number
- US04005199
Reaction notes
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