Isopropanol → HCID 22348429, compound

HRID 2244958Notes

Reaction equation

HRID 2244958 reaction equation
[Cl-].[Eu+3:2].[Cl-].[Cl-].[CH:5]([OH:8])([CH3:7])[CH3:6].[Na].[CH3:10][CH:11]([CH3:13])[O-:12].[Na+]>C1C=CC=CC=1>[CH3:6][CH:5]([CH3:7])[O-:8].[CH3:10][CH:11]([CH3:13])[O-:12].[CH3:6][CH:5]([CH3:7])[O-:8].[Eu+3:2]

Participants

6

Reactant 4

HCID 3776Isopropanol2×HCID 5360545SodiumHCID 9859933Europium chloride, anhydrous 99.9%2×HCID 109204432-Propanol, sodium salt (1:1)2×

Product 1

HCID 22348429HCID 22348429, compoundYield 95.5%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

8.60 g (28.3 mmol) of europium chloride (anhydrous) were added to a dried 250 mL round bottom flask under a nitrogen atmosphere. After the addition of 40 mL of dried isopropanol, the mixture was stirred and heated to reflux temperature. The white powders dissolved to form a clear solution. In a separate dry flask, 1.95 g (84.8 mmol) of sodium pieces was reacted with 60 mL of dried isopropanol. At the end of the reaction, the formed sodium isopropoxide was diluted with 100 mL of dried benzene. The solution was added dropwise to the europium chloride solution. The reaction took place immediately after the addition of sodium isopropoxide, as characterized by the precipitation of white sodium chloride. After the addition, the reaction mixture was stirred for an additional 2 h at boiling temperature, and then cooled to the room temperature. The mixture was allowed to stand overnight to ensure the full separation of sodium chloride. The clear top-layer was europium isopropoxide in isopropanol/benzene. The concentration of Eu(OiPr)3 is 0.1337 M (yield: about 95.5%).

Workup

  1. temperatureheated
  2. temperatureto reflux temperature
  3. dissolutionThe white powders dissolved
  4. customto form a clear solution
  5. customIn a separate dry flask
  6. customAt the end of the reaction
  7. customas characterized by the precipitation of white sodium chloride
  8. additionAfter the addition
  9. stirringthe reaction mixture was stirred for an additional 2 h
  10. customthe full separation of sodium chloride

Sources & evidence

ORD record
ord-fdd63b4641994f5ba58a5e411b36e0c4
Source dataset
uspto-grants-2010_03
Patent number
US07679082B2

Reaction notes

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