Ethanol → HCID 18931722, compound

HRID 1599194Notes

Reaction equation

HRID 1599194 reaction equation
[CH3:1][CH2:2][O-:3].[Na+].[Cl:5][CH:6]([C:11]([O:18][CH3:19])([O:16][CH3:17])[C:12]([F:15])([F:14])[F:13])C(F)(F)F.S(=O)(=O)(O)O.[CH2:25]([OH:27])[CH3:26]>>[Cl:5][CH:6]([C:11]([O:16][CH3:17])([O:18][CH3:19])[C:12]([F:13])([F:14])[F:15])[CH2:1][C:2]([O:27][CH2:25][CH3:26])=[O:3]

Participants

5

Reactant 4

HCID 702Ethanol2×HCID 1118Sulfuric AcidHCID 2723922Sodium ethoxideHCID 18931711HCID 18931711, compound

Product 1

HCID 18931722HCID 18931722, compound

Procedure

265 g of a 20% strength solution of sodium ethylate in ethanol were added dropwise to 100 g of 2-chloro-1,1,1,4,4,4-hexafluoro-3,3-dimethoxy-butane in 50 ml of ethanol at room temperature. The reaction mixture was then stirred under reflux for 12 hours and cooled to room temperature, and 100 ml of 50% strength sulfuric acid were added dropwise. After the mixture had been refluxed again for 3 hours, it was poured onto water and extracted with methylene chloride and the organic phase was dried over sodium sulfate. After removal of the solvent, the residue was distilled in vacuo.

Workup

  1. temperatureunder reflux for 12 hours
  2. temperatureAfter the mixture had been refluxed again for 3 hours
  3. additionit was poured onto water
  4. extractionextracted with methylene chloride
  5. dry with materialthe organic phase was dried over sodium sulfate
  6. customAfter removal of the solvent
  7. distillationthe residue was distilled in vacuo

Sources & evidence

ORD record
ord-da1d590ce3b64689aefbc80ab131fc6a
Source dataset
uspto-grants-1998_04
Patent number
US05739394

Reaction notes

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