Phosphoric Acid → HCID 178466060, compound

HRID 972379Notes

Reaction equation

HRID 972379 reaction equation
[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2:11].P(=O)(O)(O)[OH:13]>C(OC(=O)C)(=O)C>[C:10]([C-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1)(=[O:13])[CH3:6].[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2:11]

Participants

4

Reactant 2

HCID 1004Phosphoric AcidHCID 7611Bis(eta-cyclopentadienyl) iron

Product 1

HCID 178466060HCID 178466060, compoundYield 55.4%

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Conditions

Temperature
100 °C

Procedure

A mixture of 93.0 g (0.5 mole) of ferrocene, 250 ml of acetic anhydride and 20 ml of 85% strength phosphoric acid was heated to 100° C for 10 minutes, then cooled and poured onto ice. After leaving the mixture to stand overnight, the solid residue was filtered off and washed with water. For further purification the residue was dissolved in cyclohexane, while warming, and animal charcoal/Tonsil were added. The mixture was then filtered and the filtrate was evaporated to dryness under reduced pressure. In this way 64 g (55.4% of theory) of acetylferrocene with a melting point of 84 to 86° C were obtained.

Workup

  1. temperaturecooled
  2. additionpoured onto ice
  3. customAfter leaving the mixture
  4. filtrationthe solid residue was filtered off
  5. washwashed with water
  6. customFor further purification the residue
  7. dissolutionwas dissolved in cyclohexane
  8. temperaturewhile warming
  9. additionanimal charcoal/Tonsil were added
  10. filtrationThe mixture was then filtered
  11. customthe filtrate was evaporated to dryness under reduced pressure

Sources & evidence

ORD record
ord-e4f42bd2e2744b0d95eed075d2b7e09e
Source dataset
uspto-grants-1977_10
Patent number
US04053296

Reaction notes

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