Sulfuric Acid → HCID 86612803, compound

HRID 454785Notes

Reaction equation

HRID 454785 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[S:15](=[O:19])(=[O:18])([OH:17])O>>[F:1][C:2]1[C:3]([S:15]([OH:17])(=[O:19])=[O:18])=[CH:4][C:5]([C:8]2[CH:13]=[C:12]([S:15]([OH:17])(=[O:19])=[O:18])[C:11]([F:14])=[C:10]([S:15]([OH:17])(=[O:19])=[O:18])[CH:9]=2)=[CH:6][C:7]=1[S:15]([OH:19])(=[O:18])=[O:17]

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 98114,4'-Difluorodiphenyl

Product 1

HCID 86612803HCID 86612803, compound

Conditions

Temperature
30 °C

Procedure

The same procedure as 5a is used with 9.51 g dry 4,4′-difluorobiphenyl (50 mmole, fw=190.19) and 106.8 g 30% fuming sulfuric acid (400 mmole, fw=80.06) which are stirred at 30° C. for 24 hour and then heated with stirring at 110° C. for another 72 hours. Crystallization was effected using 29.6 g distilled water and 185 mL propionitrile. Yield was 17.2 g (65%) of the tetrasulfonated product as white crystals of the monohydrate.

Workup

  1. temperatureheated
  2. stirringwith stirring at 110° C. for another 72 hours
  3. customCrystallization
  4. distillationdistilled water and 185 mL propionitrile

Sources & evidence

ORD record
ord-5359a6cc61084a3da0713e4777fe5a34
Source dataset
uspto-grants-2013_07
Patent number
US08496835B2

Reaction notes

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