Ethane → Zinc bis(trifluoroacetate)

HRID 1494474Notes

Reaction equation

HRID 1494474 reaction equation
C([Zn:3]CC)C.[F:6][C:7]([F:12])([F:11])[C:8]([OH:10])=[O:9].CC>C1(C)C=CC=CC=1>[F:6][C:7]([F:12])([F:11])[C:8]([O-:10])=[O:9].[Zn+2:3].[F:6][C:7]([F:12])([F:11])[C:8]([O-:10])=[O:9]

Participants

5

Reactant 3

HCID 6324EthaneHCID 6422Trifluoroacetic acid2×HCID 178418750HCID 178418750, compound

Product 1

HCID 15123403Zinc bis(trifluoroacetate)

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
-40 °C

Procedure

A solution of diethyl zinc (27.5 mL, 1.1M in toluene) was slowly added to a solution of trifluoroacetic acid (2.77 mL) in dry toluene at -40° C. The reaction temp and the extent of ethane evolution was monitored. After stirring at -40° C. for 30 min, the solution was warmed to room temperature and trifluoroacetic acid (2.77 mL) was slowly added. The mixture was stirred overnight at room temperature, followed by refluxing for 2 h. A foaming suspension with a slight violet tint was formed. All volatiles were evaporated and the solid was dried at 80° C. under high vacuum. Yield: 7.65 g; 13C-NMR (75 MHz, Methanol-d4): 117.93 ppm (q, I=290.3 Hz, CF3), 163.7 ppm (q, I=36.6 Hz, CO).

Workup

  1. temperaturethe solution was warmed to room temperature
  2. stirringThe mixture was stirred overnight at room temperature
  3. temperatureby refluxing for 2 h
  4. customA foaming suspension with a slight violet tint was formed
  5. customAll volatiles were evaporated
  6. customthe solid was dried at 80° C. under high vacuum

Sources & evidence

ORD record
ord-dad0b892b28e40f094036bbf8821fbc2
Source dataset
uspto-grants-1991_06
Patent number
US05026799

Reaction notes

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