Phenol → Zirconium(2+);tetraphenoxide

HRID 745690Notes

Reaction equation

HRID 745690 reaction equation
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCCO.CCCO.CCCO.CCCO.[Zr:24]>CC1C=CC(C(C)C)=CC=1>[O-:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Zr+4:24].[O-:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O-:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O-:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 996PhenolHCID 3539967Zirconium n-propoxide

Product 1

HCID 13847644Zirconium(2+);tetraphenoxideYield 45.1%

Reagents, catalysts & solvents 1

HCID 7463P-CymeneSolvent

Procedure

Phenol (50 g), zirconium n-propoxide (10 g), and p-cymene (100 ml) were combined. The mixture was distilled through a 10 cm Vigreux column until all volatile components were removed. The cooled product was taken up in a mixture of methylene chloride (100 ml) and toluene (200 ml). This was filtered, and then concentrated under reduced pressure to a volume of ca. 50 ml. The concentrate was filtered to give 6.3 g of solid which was washed with petroleum ether, and dried under high vacuum for one hour to give white solid product.

Workup

  1. distillationThe mixture was distilled through a 10 cm Vigreux column until all volatile components
  2. customwere removed
  3. additionThe cooled product was taken up in a mixture of methylene chloride (100 ml) and toluene (200 ml)
  4. filtrationThis was filtered
  5. concentrationconcentrated under reduced pressure to a volume of ca. 50 ml
  6. filtrationThe concentrate was filtered

Sources & evidence

ORD record
ord-fc5263cc048749cba62d0ae6606dbb67
Source dataset
uspto-grants-1986_07
Patent number
US04599451

Reaction notes

Loading…