Chlorosulfonic acid → HCID 10376504, compound

HRID 618757Notes

Reaction equation

HRID 618757 reaction equation
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:8]=1[OH:14]>>[Cl:1][S:2]([C:11]1[CH:12]=[C:7]([F:6])[C:8]([OH:14])=[C:9]([F:13])[CH:10]=1)(=[O:5])=[O:3]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 943922,6-Difluorophenol

Product 1

HCID 10376504HCID 10376504, compoundYield 71.7%

Procedure

Chlorosulfonic acid (112.6 g) was added dropwise with ice cooling to 2,6-difluorophenol (25 g). The reaction mixture was stirred at room temperature for an hour and poured into ice-water (600 ml), and the separated oily substance was extracted with methylene chloride. The methylene chloride layer was washed successively with water and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give 4-chlorosulfonyl-2,6-difluorophenol (31.5 g).

Workup

  1. extractionthe separated oily substance was extracted with methylene chloride
  2. washThe methylene chloride layer was washed successively with water
  3. dry with materiala saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure

Sources & evidence

ORD record
ord-1b0f783336b746f1a6d332843c11b486
Source dataset
uspto-grants-1999_09
Patent number
US05955505

Reaction notes

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