Sodium Acetate → HCID 53785449, compound

HRID 963546Notes

Reaction equation

HRID 963546 reaction equation
[CH2:1]([O:3][C:4](=[O:19])[CH:5]([CH2:11][CH:12](Br)[CH2:13][C:14]([Cl:17])([F:16])[F:15])[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].C([O-])(=O)C.[Na+].[H][H]>[Pd].C(O)C>[CH2:1]([O:3][C:4](=[O:19])[CH:5]([CH2:11][CH2:12][CH2:13][C:14]([Cl:17])([F:16])[F:15])[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2]

Participants

6

Reactant 3

HCID 517045Sodium AcetateHCID 54490908HCID 54490908, compoundHCID 178418361HCID 178418361, compound2×

Product 1

HCID 53785449HCID 53785449, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

65.9 g of 2-(2-bromo-4-chloro-4,4-difluoro-but-1-yl)malonic acid diethyl ester, 600 ml of ethanol, 14.8 g of sodium acetate and 6.6 g of 5% palladium on activated carbon are treated with hydrogen at from 20° to 25° and under normal pressure until the absorption of hydrogen can no longer be detected. The reaction mixture is filtered over silica gel and then concentrated to dryness by evaporation in a rotary evaporator. The residue is taken up in 500 ml of n-hexane, the solution is filtered and the hexane phase is again concentrated to dryness by evaporation. The title compound is obtained in the form of a colourless oil.

Workup

  1. filtrationThe reaction mixture is filtered over silica gel
  2. concentrationconcentrated to dryness by evaporation in a rotary evaporator
  3. filtrationthe solution is filtered
  4. concentrationthe hexane phase is again concentrated to dryness by evaporation

Sources & evidence

ORD record
ord-d86956c0b10745c58cc9aeeb5f377add
Source dataset
uspto-grants-1998_06
Patent number
US05763481

Reaction notes

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