Sulfuric Acid → Sodium

HRID 1027336Notes

Reaction equation

HRID 1027336 reaction equation
[Na:1].[F:2][C:3]([F:11])([S:7]([OH:10])(=[O:9])=[O:8])[C:4]([OH:6])=[O:5].[O:12]=[C:13]1[CH:20]2[CH2:21][C:16]3(O)[CH2:17][CH:18]([CH2:22][CH:14]1[CH2:15]3)[CH2:19]2.C(C1C=CC=CC=1)C.S(=O)(=O)(O)O>>[Na:1].[F:2][C:3]([F:11])([S:7]([OH:10])(=[O:9])=[O:8])[C:4]([O:6][C:18]12[CH2:22][CH:14]3[CH2:15][CH:16]([CH2:21][CH:20]([C:13]3=[O:12])[CH2:19]1)[CH2:17]2)=[O:5]

Participants

7

Reactant 5

HCID 1118Sulfuric AcidHCID 7500EthylbenzeneHCID 64184IdramantoneHCID 654789Difluorosulfoacetic acidHCID 5360545Sodium

Product 2

HCID 5360545SodiumHCID 21111910HCID 21111910, compound

Procedure

To a mixture of 5.0 parts of sodium salt of difluorosulfoacetic acid (purity: 62.6%), 2.6 parts of 4-oxo-1-adamantanol and 100 parts of ethylbenzene, 0.6 part of concentrated sulfuric acid was added and the resultant solution was refluxed for 30 hours. The mixture was cooled and filtrated. The obtained solid was washed with tert-butyl methyl ether to obtain 5.5 parts of sodium salt of 4-oxo-1-adamantyl difluorosulfoacetate. The purity thereof was 35.6% according to 1H-NMR analysis.

Workup

  1. additionwas added
  2. temperatureThe mixture was cooled
  3. filtrationfiltrated
  4. washThe obtained solid was washed with tert-butyl methyl ether

Sources & evidence

ORD record
ord-daa6445445b24ee8ac4fcb6f015a5123
Source dataset
uspto-grants-2014_05
Patent number
US08735044B2

Reaction notes

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