3-chloro-1,1,1,4,4,4-hexafluoro-2,2-dimethoxybutane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

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. under reflux for 12 hours After the mixture had been refluxed again for 3 hours it was poured onto water extracted with methylene chloride the organic phase was dried over sodium sulfate After removal of the solvent the residue was distilled in vacuo