Chlorosulfonic acid → HCID 87147127, compound
Reaction equation
[Cl:1][S:2]([OH:5])(=O)=[O:3].[Cl:6][C:7]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:8]=1[C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:10]>>[Cl:6][C:7]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:8]=1[C:9]([C:11]1[CH:16]=[C:15]([S:2]([Cl:1])(=[O:5])=[O:3])[CH:14]=[CH:13][CH:12]=1)=[O:10]Participants
3
Procedure
Chlorosulfonic acid (233.0 g, 2 mol) was added into a 3 L three-necked flask equipped with a stirrer and cooling pipe, followed by adding 2,5-dichlorobenzophenone (100.4 g, 400 mmol), and the reactant was allowed to react for 8 hours using an oil bath at 100° C. After a predetermined time, the reaction liquid was slowly poured into crushed ice (1000 g) and extracted with ethyl acetate. The organic layer was washed with sodium chloride solution and dried with magnesium sulfate, and then ethyl acetate was removed to obtain a light yellow crude crystal (3-(2,5-dichlorobenzoyl)benzenesulfonic acid chloride. The crude crystal was not purified and directly used in the following step.
Workup
- customequipped with a stirrer
- temperaturecooling pipe
- customto react for 8 hours
- customat 100° C
- customAfter a predetermined time, the reaction liquid
- additionwas slowly poured
- extractionextracted with ethyl acetate
- washThe organic layer was washed with sodium chloride solution
- dry with materialdried with magnesium sulfate
- customethyl acetate was removed
Sources & evidence
- ORD record
- ord-826b27c7e1274c3bb1ce13ff174e21a6
- Source dataset
- uspto-grants-2012_09
- Patent number
- US08273499B2
Reaction notes
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