Sulfuric Acid → HCID 86612802, compound
Reaction equation
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:4][C:3]=1[C:15]([OH:17])=[O:16].[S:18](=[O:22])(=[O:21])([OH:20])O>>[C:15]([C:3]1[CH:4]=[C:5]([C:8]2[CH:13]=[C:12]([S:18]([OH:20])(=[O:22])=[O:21])[C:11]([CH3:14])=[C:10]([S:18]([OH:22])(=[O:21])=[O:20])[CH:9]=2)[CH:6]=[C:7]([S:18]([OH:20])(=[O:22])=[O:21])[C:2]=1[OH:1])([OH:17])=[O:16]Participants
3
Conditions
- Temperature
- 30 °C
Procedure
The same procedure as 5a is used with 11.42 g dry 4-hydroxy-4′-methylbiphenyl-3-carboxylic acid (50 mmole, fw=228.25) and 80.1 g 30% fuming sulfuric acid (300 mmole, fw=80.06) which are stirred at 30° C. for 24 hour and then heated with stirring at 70° C. for another 24 hours. Crystallization was effected using 22.2 g distilled water and 145 mL propionitrile. Yield was 21.2 g (84%) of the trisulfonated product as white crystals of the dihydrate.
Workup
- temperatureheated
- stirringwith stirring at 70° C. for another 24 hours
- customCrystallization
- distillationdistilled water and 145 mL propionitrile
Sources & evidence
- ORD record
- ord-615a7aeaf65943be82fe8751f4e77cb7
- Source dataset
- uspto-grants-2013_07
- Patent number
- US08496835B2
Reaction notes
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