Phosphoric Acid → HCID 178466060, compound

HRID 1577572Notes

Reaction equation

HRID 1577572 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 mol) 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 added to ice. After standing overnight, the solid residue was filtered off and washed with water. For further purification, the residue was dissolved in cyclohexane, while warming, animal charcoal/Tonsil being added. The mixture was then filtered and the filtrate was evaporated to dryness under reduced pressure. 64 g (55.4% of theory) of acetylferrocene of melting point 84°-86° C. were obtained in this manner.

Workup

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

Sources & evidence

ORD record
ord-ea0fd05ce6944676957a5357a3274ea2
Source dataset
uspto-grants-1981_09
Patent number
US04288451

Reaction notes

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