Sodium Acetate → HCID 19801961, compound

HRID 1646267Notes

Reaction equation

HRID 1646267 reaction equation
Cl[C:2](Cl)([CH2:8][C:9]([Cl:12])([F:11])[F:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].C([O-])(=O)C.[Na+].[H][H]>C(O)C.[Pt]>[Cl:12][C:9]([F:10])([F:11])[CH2:8][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4]

Participants

6

Reactant 3

HCID 517045Sodium AcetateHCID 19801958Ethyl 2,2,4-trichloro-4,4-difluorobutanoateHCID 178418361HCID 178418361, compound2×

Product 1

HCID 19801961HCID 19801961, compoundYield 75.2%

Reagents, catalysts & solvents 2

HCID 23939PlatinumCatalystHCID 702EthanolSolvent

Procedure

25.5 g of ethyl 2,2,4-trichloro-4,4-difluorobutyrate are dissolved in 200 ml of absolute ethanol. 16.4 g of anhydrous sodium acetate and 2.0 g of 5% platinum/carbon catalyst are added and then gaseous hydrogen is passed in under atmospheric pressure until the hydrogen uptake is 2 equivalents. The catalyst is removed by filtration and the ethanol is removed by distillation and then the remaining oil is poured onto water, and the organic phase is separated off, dried with sodium sulfate, filtered and distilled under atmospheric pressure. 14.0 g of ethyl 4-chloro-4,4-difluorobutyrate are obtained in the form of a colourless oil of boiling point 154°-156° C.

Workup

  1. customThe catalyst is removed by filtration
  2. customthe ethanol is removed by distillation
  3. additionthe remaining oil is poured onto water
  4. customthe organic phase is separated off
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. distillationdistilled under atmospheric pressure

Sources & evidence

ORD record
ord-07e737889c084c39a4af8c33ba0363ce
Source dataset
uspto-grants-1993_01
Patent number
US05179121

Reaction notes

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