Reaction #1772002

ord-dac40518dff544c4a0e9bacff6546e56

Reaction equation

CCOCC
diethyl ether
FC(F)(F)C(F)(Cl)Cl
CFC-114a
Cl
hydrochloric acid
OCC(F)(Cl)C(F)(F)F
CF3CClFCH2OH

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONby diluting the reaction product mixture
  2. 2
    workup.ADDITIONwith a mixture of a solvent, ice
  3. 3
    Otheris separated
  4. 4
    WashThe organic solvent layer can be subsequently washed with a dilute aqueous solution of an acid
  5. 5
    OtherThe organic layer is then dried
  6. 6
    workup.STIRRINGby stirring the organic layer over an anhydrous salt
  7. 7
    OtherThe organic solvent may then be evaporated

Procedure

The reaction product of CFC-114a, an aldehyde and a reactive metal may be neutralized by diluting the reaction product mixture with a mixture of a solvent, ice, and an aqueous solution of an acid. The solvent can be any commonly used organic solvent, such as diethyl ether. The aqueous solution of an acid may be an aqueous solution of a common mineral acid, such as hydrochloric acid. After stirring the resulting mixture for a period of time, the layer comprising the organic solvent is separated. The organic solvent layer can be subsequently washed with a dilute aqueous solution of an acid, followed by a brine solution. The organic layer is then dried. The drying is accomplished by stirring the organic layer over an anhydrous salt, such as anhydrous magnesium sulfate or anhydrous sodium sulfate. The organic solvent may then be evaporated to afford CF3CClFCH2OH.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08147710B2uspto-grants-2012_04